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WillD

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Reaction scheme:
NZ1iBTbJUl
Reagents:
  • Indole (cas 120-72-9) 0.117 g;
  • Aluminum oxide (Al2O3) 1 g;
  • 1-Naphthoyl chloride (cas 879-18-5) 0.286 g;
  • Sodium carbonate (Na2CO3) 0.16 g;
  • 1-Bromopentane (cas 110-53-2) 0.18 g;
  • Ethanol (EtOH) 60 ml;
  • Distilled water;

Equipment and glassware:
  • Microwave vial 5 ml;
  • Microwave oven;
  • Beakers 10 mL x2;
  • Glass rod and spatula;
  • Heating plate;
  • Freezer;
  • Vacuum source (optional);
  • Schott filter and Buchner flask (optional);

Synthesis:
1. Indole 0.117 g is mixed with aluminum oxide (Al2O3) 1 g and mixed together until a homogeneous powder is formed.
2. 1-Naphthoyl chloride 0.286 g is added to the mixture and stirred to evenly mixed solution.
3. The final mixture is irradiated at 100 °С (400 W) for 8 minutes in a sealed 5 ml microwave vial.
4. The vial is cooled to a room temperature. Sodium carbonate (Na2CO3) 0.16 g as a finely ground powder and 1-bromo-pentane 0.18 g are added into the vial and then stirred to evenly mixed solution.
5. The resulting mixture is irradiated again in the microwave reactor (vial) at 100 °C (400W) for 4 minutes.
6. Then, ethanol (EtOH) 60 ml is added to the reaction mixture and
refluxed for 20 minutes.
7. Aluminum oxide (Al2O3) is filtered and washed with distilled water 15 ml twice, and dried for next batch.
8. Ethanol solution (EtOH) with JWH-018 is treated with water 10 ml, placed in a freezer and crystalline JWH-018 is formed. Product is
filtered on a Schott funnel and Buchner flask.

JWH-018 can be used as liquid.
 
Last edited by a moderator:

jexana23

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I m a novice , can you explainbetter, i search for indole and i found many tipes of indole and my brain go down :)
How much quantyti etc.
 
Last edited:

jexana23

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Reaction scheme:
View attachment 1666
Synthesis:
1. Indole (0,117 g) was mixed with neutral Al2O3 (1 g) and ground together until a homogeneous powder was formed.
2. 1-naphthoyl chloride (0,286 g) was added to the mixture and stirred to homogeneity.
3. The final mixture in a sealed 5 ml microwave vial was subjected to irradiation in a microwave reactor at 100 *C (400 W) for 8 minutes.
4. After cooling to room temperature, 0,16 g of Na2CO3 as a finely ground powder and 0,18 g of 1-bromo-pentane were added into the microwave vial and then stirred to homogeneity.
5. The resulting mixture was irradiated again in the microwave reactor at 100*C (400W) for 4 minutes.
6. Then, 60 ml EtOH was added to the reaction mixture and refluxed for 20 minutes.
7. Al2O3 was filtered and washed with 15 ml water twice, and dried for a next cycle.
8. The EtOH phase was treated with a solution of 10 ml water, after which a solid was formed.
William DampierCan you explain for stupit noob people like me , i know i m very stupid but if you explain for noobs i think it a possible to understand
 

nutritiousforeach

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Reaction scheme:
View attachment 1666
Synthesis:
1. Indole (0,117 g) was mixed with neutral Al2O3 (1 g) and ground together until a homogeneous powder was formed.
2. 1-naphthoyl chloride (0,286 g) was added to the mixture and stirred to homogeneity.
3. The final mixture in a sealed 5 ml microwave vial was subjected to irradiation in a microwave reactor at 100 *C (400 W) for 8 minutes.
4. After cooling to room temperature, 0,16 g of Na2CO3 as a finely ground powder and 0,18 g of 1-bromo-pentane were added into the microwave vial and then stirred to homogeneity.
5. The resulting mixture was irradiated again in the microwave reactor at 100*C (400W) for 4 minutes.
6. Then, 60 ml EtOH was added to the reaction mixture and refluxed for 20 minutes.
7. Al2O3 was filtered and washed with 15 ml water twice, and dried for a next cycle.
8. The EtOH phase was treated with a solution of 10 ml water, after which a solid was formed.
William Dampier
Why is irradiation specifically used, instead of normal controlled heating at 100*C? Just wanted to understand the chemistry. Thank you.
 

krtl91

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hi there . thank you for information. what can i use instead of 1 naphtoyl chloride ? i cant find it commercially here . or how can i make for my self ? thx
 

WillD

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hi there . thank you for information. what can i use instead of 1 naphtoyl chloride ? i cant find it commercially here . or how can i make for my self ? thx
krtl911-naphthoyl chloride substituted - 4-methoxy or 4-ethyl -1-naphthoyl chlorides. 1-Adamantanecarbonyl chloride, 2-Iodobenzoyl chloride, 2,2,3,3-Tetramethylcyclopropanecarbonyl chloride, etc
 

krtl91

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thank you so much
 

krtl91

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is there one which i could find commercially available easier than others ? thank you
 

krtl91

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1-naphthoyl chloride substituted - 4-methoxy or 4-ethyl -1-naphthoyl chlorides. 1-Adamantanecarbonyl chloride, 2-Iodobenzoyl chloride, 2,2,3,3-Tetramethylcyclopropanecarbonyl chloride, etc
William Dampierhi there .Thank you for your time . İ am having trouble to find those reagents commercially available. Which one of those i can synthesis myself from the commercially available ones (as a amateur one i would prefer to easiest one ) thank you :) .
 

WillD

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You can find acid, not chloride (for example naphthoyl acid) and make chloride with thionyl chloride or phosphoryl chloride. Synthesis (click). You can use other acids, by analogy.
 

krtl91

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You can find acid, not chloride (for example naphthoyl acid) and make chloride with thionyl chloride or phosphoryl chloride. Synthesis (click). You can use other acids, by analogy.
William Dampiernone of them İ mean literally none of them available commercially in my frkng country. ı guess ı ll just order napthoyl cloride from chına or somewhere and do the procedure . coz ı assume as a amateur ıt doesnt worth to that much trouble to optaın naphtoyl chlorıde when ıts avaılable commercially ın other countrıes
 

WillD

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Yes, of course it is better to buy chloride than to make it, not the most pleasant procedure.
 

northenos

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What equipment needed to microwave synthesis ?
 

WillD

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MW oven, beakers, scales, grinders, filters, etc.
PS: Who synthesizes ADBB-noids with main reagent (with potassium carbonate), can try this synthesis starting from step 4
 

northenos

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I still confused start step 6, what equipment needed to reflux ?
any video to explain that ?
 

northenos

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After reflux, the mixture filtered and the filter washed with water twice ? How to wash that i need example, and step 8 i still confused with the word “EtOH phase”, what is EtOH phase ?
 
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