Background and overview[1]
4-Chlorobutanone can be used as a pharmaceutical synthesis intermediate. If 4-chlorophenbutanone is inhaled, move the patient to fresh air; if the skin comes into contact, take off contaminated clothing, rinse the skin thoroughly with soap and water, and seek medical treatment if you feel uncomfortable; if the eye contacts, remove the contaminated clothing. The eyelids should be separated, rinsed with running water or saline, and seek medical attention immediately; if ingested, rinse mouth immediately, do not induce vomiting, and seek medical attention immediately.
Preparation[1]
The preparation of 4-chlorophenylbutanone is as follows:
The specific steps are as follows: Add 500ml of chlorobenzene and 1.0mol of aluminum trichloride into the three-necked flask, cool the temperature to 0°C, and begin to slowly add 1mol of n-butyroyl chloride dropwise at a rate of 1.5mL/min. After the dropwise addition is completed, keep it warm. React for 3 hours, then raise the temperature to 25°C and keep it for 30 hours. After GC detects that the reaction is complete, hydrolyze. During hydrolysis, slowly pour the reaction solution into 300ml of 10% dilute hydrochloric acid ice-water mixture, keep the hydrolysis temperature not exceeding 60°C, and stir 30min, then let it stand for 60min for layering. Take the oil phase and wash it twice with 200ml of water. The stirring time is 30min and the standing time is 60min for layering. The resulting oil phase contains 4-chlorophenylbutanone.
Application
4-Chlorobutanone can be used as a pharmaceutical synthesis intermediate. If bromination reaction occurs:
Add 1 mol of hydrogen peroxide to the oil phase of 4-chlorophenylbutanone, add 0.5 mol of bromine dropwise at room temperature, incubate for 0.5 hours, and detect by GC. After Compound I has completely reacted, hydrolyze it. During hydrolysis, the reaction solution was slowly Pour 300ml of water, keep the hydrolysis temperature not exceeding 60°C, stir for 30 minutes, and then let it stand for 60 minutes to separate layers. Take the oil phase and wash it twice with 200ml of water. Stir for 30 minutes and let stand for 60 minutes to separate layers. The resulting organic phase goes into the next step. step process.
Main reference materials
[1]CN201810101272.9 A synthesis method of 2-benzyl-2-dimethylamino-1-(4-morpholinophenyl)butanone
微信扫一扫打赏
