Reaction scheme:
Reagents:
Synthesis:
Reagents:
- 4'-Methylpropiophenone (cas 5337-93-9) 5 kg;
- Сooper(II) oxide (CuO) 2.7 kg;
- Isopropyl alcohol (IPA) 50 l;
- Iodine 6.5 kg;
- 100 L Batch reactor, which is equipped with drip funnel, top stirrer, thermometer, temperature control system (cooling) and reflux condenser;
- Funnel;
- Several buckets 25 L or more;
- Barrel 100 L;
- Beaker 2000 mL;
- Vacuum source;
- Scale;
- Measuring cylinder 1000 mL;
- Glass rod and spatula;
- Scoops;
- Nutsche filter;
- Rotary evaporator;
- Shovel;
Synthesis:
1. 4'-Methylpropiophenone 5 kg and IPA 50 l are added into a 100 L batch reactor.
2. Stirrer is turned on.
3. Сooper(II) oxide fine powder 2.7 kg is slowly added to the mixture with a stirring.
4. Iodine (I2) 6.5 kg is added to the mixture with stirring as well.
5. The reaction mixture is heated to 70 °C, then reaction is left for 24 h with a constant stirring and heating.
6. After, the stirrer is turned off. The solution is left to precipitate copper. The heating is continued.
7. 2-Iodo-4'-methylpropiophenone solution is decanted from precipitate through a top of the reactor.
8. The solution is put into a freezer for 24 h.
9. 2-Iodo-4'-methylpropiophenone crystals are filtered through a nutsche filter, washed with cold IPA on the filter.
10. Filtered solution 2/3 is distilled off in rotovap, crystallized and washed again.
11. 2-Iodo-4'-methylpropiophenone crystals are dried under vacuum or on air. Yield is 6.5 kg.
2. Stirrer is turned on.
3. Сooper(II) oxide fine powder 2.7 kg is slowly added to the mixture with a stirring.
4. Iodine (I2) 6.5 kg is added to the mixture with stirring as well.
5. The reaction mixture is heated to 70 °C, then reaction is left for 24 h with a constant stirring and heating.
6. After, the stirrer is turned off. The solution is left to precipitate copper. The heating is continued.
7. 2-Iodo-4'-methylpropiophenone solution is decanted from precipitate through a top of the reactor.
8. The solution is put into a freezer for 24 h.
9. 2-Iodo-4'-methylpropiophenone crystals are filtered through a nutsche filter, washed with cold IPA on the filter.
10. Filtered solution 2/3 is distilled off in rotovap, crystallized and washed again.
11. 2-Iodo-4'-methylpropiophenone crystals are dried under vacuum or on air. Yield is 6.5 kg.
2-Iodo-4'-methylpropiophenone synthesis (cas 236117-38-7)
- Three-necked round bottom flask 2000 mL;
- Stirrer with heating surface and water bath;
- Schott funnel and Buchner flask;
- Beakers;
- Scale;
- Measuring cylinder 100 mL;
- 4'-Methylpropiophenone (4-MP; cas 5337-93-9) 100 g;
- Iodine (I2) 128 g;
- Isopropyl alcohol (IPA) 1000 mL;
- Сooper(II) oxide (CuO) 53 g;
(00:50) - Distilled water is poured into the water bath vessel, immerse approximately half of the round bottom flask in water. Better to immerse the flask with reaction mixture (Rm) level in the same level of water in the bath.
(01:07) - Set the heater temperature to 80 °C. The water temperature have to be >60 °C. Reagents are added to the flask one by one when the water temperature reaches 60 °C.
4-MP (100 g) + IPA (1000 mL) and turn on the stirrer.
(2:00) - Copper oxide (CuO) 53 g is added to Rm through the powder funnel.
Copper oxide (CuO) have to be distributed throughout the Rm volume with stirring.
(2:22) - Next, dry Iodine 128 g is added in several portions. Fraction of Iodine does not matter (granular or crystalline).
Iodine is dissolved in IPA. Remember that Iodine is a halogen and an exhaust ventilation have to be used in safety reasons.
(2:46) - Reflux condenser (with cold water flow) is attached to the a round bottom flask in order to condense reaction vapors.
An insoluble CuO suspension and Iodine are observed in Rm, which should uniformly fill all reaction volume by stirring. Otherwise, the reaction will be carried out incorrectly.
(3:11) - Changes in Rm is observed after 15-20 h from the reaction start. The reaction can be carried out at this temperature regime for a longer time, but not less than 15 hours.
(3:30) - The stirrer is turned off. Copper compounds have to be precipitated in entire solution volume.
(3:38) - Rm is decanted. Copper precipitates are left in the vessel. The precipitate is disposed.
(3:52) - Rm is alcohol solution of 2-Iodo-4'-methylpropiophenone. It is cooled at room temperature, and then put into a freezer for 12 hours.
(4:00) - 2-Iodo-4'-methylpropiophenone is crystallized in a beaker. A suction filter system is prepared and IPA (to wash the crystallized product) is cooled in the freezer.
(4:27) - 2-Iodo-4'-methylpropiophenone is filtered, washed with chilled IPA, dried to a constant weight at room temperature under vacuum (optional).
(4:45) - 2-Iodo-4'-methylpropiophenone (cas 236117-38-7) final yield is 130 g.
(01:07) - Set the heater temperature to 80 °C. The water temperature have to be >60 °C. Reagents are added to the flask one by one when the water temperature reaches 60 °C.
4-MP (100 g) + IPA (1000 mL) and turn on the stirrer.
(2:00) - Copper oxide (CuO) 53 g is added to Rm through the powder funnel.
Copper oxide (CuO) have to be distributed throughout the Rm volume with stirring.(2:22) - Next, dry Iodine 128 g is added in several portions. Fraction of Iodine does not matter (granular or crystalline).
Iodine is dissolved in IPA. Remember that Iodine is a halogen and an exhaust ventilation have to be used in safety reasons.(2:46) - Reflux condenser (with cold water flow) is attached to the a round bottom flask in order to condense reaction vapors.
An insoluble CuO suspension and Iodine are observed in Rm, which should uniformly fill all reaction volume by stirring. Otherwise, the reaction will be carried out incorrectly.(3:11) - Changes in Rm is observed after 15-20 h from the reaction start. The reaction can be carried out at this temperature regime for a longer time, but not less than 15 hours.
(3:30) - The stirrer is turned off. Copper compounds have to be precipitated in entire solution volume.
(3:38) - Rm is decanted. Copper precipitates are left in the vessel. The precipitate is disposed.
(3:52) - Rm is alcohol solution of 2-Iodo-4'-methylpropiophenone. It is cooled at room temperature, and then put into a freezer for 12 hours.
(4:00) - 2-Iodo-4'-methylpropiophenone is crystallized in a beaker. A suction filter system is prepared and IPA (to wash the crystallized product) is cooled in the freezer.
(4:27) - 2-Iodo-4'-methylpropiophenone is filtered, washed with chilled IPA, dried to a constant weight at room temperature under vacuum (optional).
(4:45) - 2-Iodo-4'-methylpropiophenone (cas 236117-38-7) final yield is 130 g.
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