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- Sep 3, 2023
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## **Step-by-Step Synthesis**
### **Part 1: Conversion of BMK Glycidic Acid Sodium Salt to P2P**
#### Materials:
- **500 g of BMK Glycidic Acid Sodium Salt**
- **500 mL of boiling water** (for dissolving the sodium salt)
- **600 mL of 85% phosphoric acid** (for the reaction)
#### Equipment:
- **2 L reaction flask**
- **Dropping funnel**
- **Reflux apparatus**
- **Steam distillation setup**
#### Procedure:
1. **Dissolve 500 g of BMK Glycidic Acid Sodium Salt** in **500 mL of boiling water**.
2. In a **2 L reaction flask**, add **600 mL of 85% phosphoric acid** and begin heating the flask to a temperature of **100–120°C**.
3. Using a **dropping funnel**, slowly add the **BMK Glycidic Acid Sodium Salt solution** into the boiling phosphoric acid.
This should take about **1–2 hours**.
4. After the complete addition of the sodium salt solution, allow the reaction mixture to reflux at **100–120°C** for an additional **1–2 hours** to ensure full conversion to **P2P**.
5. After reflux, let the mixture cool slightly, then perform **steam distillation** to isolate **P2P** from the reaction mixture.
6. The P2P will collect in the receiving flask with water. Separate the P2P layer from the water layer.
### **: Steam Distillation of P2P**
#### Materials:
- **250 mL of P2P**
- **500 mL of water**
- **75 g of potassium carbonate (K₂CO₃)**
- **Silica gel** for drying
#### Procedure:
1. In a **1 L distillation flask**, add **250 mL of P2P**, **Dissolve the 75g Potassium Carbonate (K₂CO₃) in 500mL of water**, and add the 75g Potassium Carbonate (K₂CO₃) solution to the distillation flask**.
2. Set up for **steam distillation**. Steam distill the mixture, collecting P2P in the receiving flask.
3. Once distillation is complete, you will have **P2P oil** mixed with water in the receiving flask.
4. Separate the oil from the water layer using a **separatory funnel**.
Use a 100g sodium chloride + 500ml H2O add it to the Separatory Funnel it will make all the P2P oil float on top!
5. **Dry 325ml of P2P over 32.5g of silica gel for ~2 hours~**.
#### Expected Yield:
- From **500 g of BMK Glycidic Acid Sodium Salt**, you should expect around **325 mL of pure P2P**.
---
### **Part 2: Leuckart-Wallach Reaction (P2P to N-Formylamphetamine)**
#### Materials:
- **250 mL of P2P** (pure)
- **375 mL of formamide** (1.5 mol equivalents)
- **175–200 mL of formic acid** (1.1 mol equivalents)
- **10.2 g of zinc chloride (ZnCl₂)** (catalyst)
- **333.25 mL of water** (for layer separation)
- **DCM (dichloromethane)** (for extraction)
- **Anhydrous sodium sulfate (Na₂SO₄)** or **magnesium sulfate (MgSO₄)** for drying
#### Equipment:
- **Reflux setup** with heating and stirring
- **Separatory funnel**
#### Procedure:
1. In a **2 L reaction flask**, add **250 mL of pure P2P**, **375 mL of formamide**, **175–200 mL of formic acid**, and **10.2 g of zinc chloride (ZnCl₂)**.
2. Heat the mixture to **140–150°C** and reflux for **5 hours**, stirring continuously.
3. After 5 hours, stop heating and allow the mixture to cool down to a safe temperature to add H2O without a big evaporation.
4. Add **333.25 mL of water** to the mixture, being careful of any evaporation.
5. The mixture will separate into two layers:
- The **top oil layer** contains **N-Formylamphetamine**.
- The **bottom aqueous layer** contains byproducts.
6. In a **separatory funnel**, separate the top oil layer and keep it aside.
7. Extract the bottom aqueous layer with **DCM** (dichloromethane). Combine the DCM layer with the oil layer.
8. Dry the combined layers with **anhydrous Na₂SO₄ or MgSO₄**, then filter and evaporate the DCM to yield **N-Formylamphetamine**.
#### Expected Yield:
- You should obtain approximately **275 mL of N-Formylamphetamine** from **250 mL of P2P**.
---
### **Part 3: Hydrolysis of N-Formylamphetamine with HCL to Amphetamine Freebase Oil**
#### Materials:
- **275 mL of N-Formylamphetamine**
- **Concentrated HCl (37%)** for hydrolysis
- **DCM (dichloromethane)** for extraction
- **Anhydrous Na₂SO₄ or MgSO₄** for drying
#### Procedure:
1. Add **275 mL of N-Formylamphetamine** to a reaction flask and carefully add **concentrated HCl** to hydrolyze the formyl group, forming **amphetamine freebase oil**.
2. Extract the amphetamine freebase oil using **DCM**. Separate the organic (DCM) layer and dry it with **anhydrous Na₂SO₄ or MgSO₄**.
3. Filter and evaporate the DCM to yield **amphetamine freebase oil**.
### Hydrolysis of N-Formylamphetamine (NaOH or KOH Route) to Amphetamine Freebase Oil:
1. **KOH or NaOH solution 50%. 227.5 g of KOH to have the same effect as 162.5 g of NaOH and fill up till 325ml H2O mixture.
2. **Hydrolysis reactions with KOH or NaOH are conducted around 90–100°C. slow stirring with reflux during 2-3 hours.
#### Expected Yield:
- You should yield approximately **225–250 mL of amphetamine freebase oil**.
---
### **Part 4: Steam Distillation of Amphetamine Freebase Oil**
#### Materials:
- **250 mL of amphetamine freebase oil**
- **500 mL of water**
- **Silica gel** for drying
#### Procedure:
1. In a **1 L distillation flask**, add **250 mL of amphetamine freebase oil** and **500 mL of water**.
2. Set up for **steam distillation**. Steam distill the mixture, collecting the amphetamine freebase oil in the receiving flask.
3. Once distillation is complete, you will have **amphetamine freebase oil** mixed with water in the receiving flask.
4. Separate the oil from the water layer using a **separatory funnel**.
#### Drying the Freebase Oil:
1. To dry **100 mL of amphetamine freebase oil**, you will need about **50–100 g of silica gel**.
2. Add the amphetamine freebase oil to a flask containing **silica gel** and allow it to sit for **2–4 hours**, stirring occasionally.
3. Once dried, decant the amphetamine freebase oil.
#### Expected Yield:
- After steam distillation, you should yield approximately **225–250 mL of pure amphetamine freebase oil** from the **250 mL of P2P** used in the Leuckart-Wallach reaction.
---
### **Overall Yields**
1. **BMK Glycidic Acid Sodium Salt to P2P**: Approx. **325 mL of pure P2P** from **500 g of sodium salt**.
2. **Leuckart-Wallach Reaction (P2P to N-Formylamphetamine)**: Approx. **275 mL of N-Formylamphetamine** from **250 mL of P2P**.
3. **Hydrolysis of N-Formylamphetamine**: Approx. **225–250 mL of amphetamine freebase oil**.
4. **Final steam distillation**: Recover **225–250 mL** of purified amphetamine freebase oil.
This complete synthesis includes all steps from the conversion of sodium salt to P2P, through the Leuckart-Wallach reaction, and the final steam distillation and drying of amphetamine freebase oil.
### **Part 1: Conversion of BMK Glycidic Acid Sodium Salt to P2P**
#### Materials:
- **500 g of BMK Glycidic Acid Sodium Salt**
- **500 mL of boiling water** (for dissolving the sodium salt)
- **600 mL of 85% phosphoric acid** (for the reaction)
#### Equipment:
- **2 L reaction flask**
- **Dropping funnel**
- **Reflux apparatus**
- **Steam distillation setup**
#### Procedure:
1. **Dissolve 500 g of BMK Glycidic Acid Sodium Salt** in **500 mL of boiling water**.
2. In a **2 L reaction flask**, add **600 mL of 85% phosphoric acid** and begin heating the flask to a temperature of **100–120°C**.
3. Using a **dropping funnel**, slowly add the **BMK Glycidic Acid Sodium Salt solution** into the boiling phosphoric acid.
This should take about **1–2 hours**.
4. After the complete addition of the sodium salt solution, allow the reaction mixture to reflux at **100–120°C** for an additional **1–2 hours** to ensure full conversion to **P2P**.
5. After reflux, let the mixture cool slightly, then perform **steam distillation** to isolate **P2P** from the reaction mixture.
6. The P2P will collect in the receiving flask with water. Separate the P2P layer from the water layer.
### **: Steam Distillation of P2P**
#### Materials:
- **250 mL of P2P**
- **500 mL of water**
- **75 g of potassium carbonate (K₂CO₃)**
- **Silica gel** for drying
#### Procedure:
1. In a **1 L distillation flask**, add **250 mL of P2P**, **Dissolve the 75g Potassium Carbonate (K₂CO₃) in 500mL of water**, and add the 75g Potassium Carbonate (K₂CO₃) solution to the distillation flask**.
2. Set up for **steam distillation**. Steam distill the mixture, collecting P2P in the receiving flask.
3. Once distillation is complete, you will have **P2P oil** mixed with water in the receiving flask.
4. Separate the oil from the water layer using a **separatory funnel**.
Use a 100g sodium chloride + 500ml H2O add it to the Separatory Funnel it will make all the P2P oil float on top!
5. **Dry 325ml of P2P over 32.5g of silica gel for ~2 hours~**.
#### Expected Yield:
- From **500 g of BMK Glycidic Acid Sodium Salt**, you should expect around **325 mL of pure P2P**.
---
### **Part 2: Leuckart-Wallach Reaction (P2P to N-Formylamphetamine)**
#### Materials:
- **250 mL of P2P** (pure)
- **375 mL of formamide** (1.5 mol equivalents)
- **175–200 mL of formic acid** (1.1 mol equivalents)
- **10.2 g of zinc chloride (ZnCl₂)** (catalyst)
- **333.25 mL of water** (for layer separation)
- **DCM (dichloromethane)** (for extraction)
- **Anhydrous sodium sulfate (Na₂SO₄)** or **magnesium sulfate (MgSO₄)** for drying
#### Equipment:
- **Reflux setup** with heating and stirring
- **Separatory funnel**
#### Procedure:
1. In a **2 L reaction flask**, add **250 mL of pure P2P**, **375 mL of formamide**, **175–200 mL of formic acid**, and **10.2 g of zinc chloride (ZnCl₂)**.
2. Heat the mixture to **140–150°C** and reflux for **5 hours**, stirring continuously.
3. After 5 hours, stop heating and allow the mixture to cool down to a safe temperature to add H2O without a big evaporation.
4. Add **333.25 mL of water** to the mixture, being careful of any evaporation.
5. The mixture will separate into two layers:
- The **top oil layer** contains **N-Formylamphetamine**.
- The **bottom aqueous layer** contains byproducts.
6. In a **separatory funnel**, separate the top oil layer and keep it aside.
7. Extract the bottom aqueous layer with **DCM** (dichloromethane). Combine the DCM layer with the oil layer.
8. Dry the combined layers with **anhydrous Na₂SO₄ or MgSO₄**, then filter and evaporate the DCM to yield **N-Formylamphetamine**.
#### Expected Yield:
- You should obtain approximately **275 mL of N-Formylamphetamine** from **250 mL of P2P**.
---
### **Part 3: Hydrolysis of N-Formylamphetamine with HCL to Amphetamine Freebase Oil**
#### Materials:
- **275 mL of N-Formylamphetamine**
- **Concentrated HCl (37%)** for hydrolysis
- **DCM (dichloromethane)** for extraction
- **Anhydrous Na₂SO₄ or MgSO₄** for drying
#### Procedure:
1. Add **275 mL of N-Formylamphetamine** to a reaction flask and carefully add **concentrated HCl** to hydrolyze the formyl group, forming **amphetamine freebase oil**.
2. Extract the amphetamine freebase oil using **DCM**. Separate the organic (DCM) layer and dry it with **anhydrous Na₂SO₄ or MgSO₄**.
3. Filter and evaporate the DCM to yield **amphetamine freebase oil**.
### Hydrolysis of N-Formylamphetamine (NaOH or KOH Route) to Amphetamine Freebase Oil:
1. **KOH or NaOH solution 50%. 227.5 g of KOH to have the same effect as 162.5 g of NaOH and fill up till 325ml H2O mixture.
2. **Hydrolysis reactions with KOH or NaOH are conducted around 90–100°C. slow stirring with reflux during 2-3 hours.
#### Expected Yield:
- You should yield approximately **225–250 mL of amphetamine freebase oil**.
---
### **Part 4: Steam Distillation of Amphetamine Freebase Oil**
#### Materials:
- **250 mL of amphetamine freebase oil**
- **500 mL of water**
- **Silica gel** for drying
#### Procedure:
1. In a **1 L distillation flask**, add **250 mL of amphetamine freebase oil** and **500 mL of water**.
2. Set up for **steam distillation**. Steam distill the mixture, collecting the amphetamine freebase oil in the receiving flask.
3. Once distillation is complete, you will have **amphetamine freebase oil** mixed with water in the receiving flask.
4. Separate the oil from the water layer using a **separatory funnel**.
#### Drying the Freebase Oil:
1. To dry **100 mL of amphetamine freebase oil**, you will need about **50–100 g of silica gel**.
2. Add the amphetamine freebase oil to a flask containing **silica gel** and allow it to sit for **2–4 hours**, stirring occasionally.
3. Once dried, decant the amphetamine freebase oil.
#### Expected Yield:
- After steam distillation, you should yield approximately **225–250 mL of pure amphetamine freebase oil** from the **250 mL of P2P** used in the Leuckart-Wallach reaction.
---
### **Overall Yields**
1. **BMK Glycidic Acid Sodium Salt to P2P**: Approx. **325 mL of pure P2P** from **500 g of sodium salt**.
2. **Leuckart-Wallach Reaction (P2P to N-Formylamphetamine)**: Approx. **275 mL of N-Formylamphetamine** from **250 mL of P2P**.
3. **Hydrolysis of N-Formylamphetamine**: Approx. **225–250 mL of amphetamine freebase oil**.
4. **Final steam distillation**: Recover **225–250 mL** of purified amphetamine freebase oil.
This complete synthesis includes all steps from the conversion of sodium salt to P2P, through the Leuckart-Wallach reaction, and the final steam distillation and drying of amphetamine freebase oil.