反应详情

温度

0 °C

This product is obtained according to Sugasawa T., Toyoda T., Adachi M., Sasakura K., J. Am. Chein. Soc., 100 (1978), p. 4842-4852). A molar solution of boron trichloride in hexane (164 ml, 164 mmol), chloroacetonitrile (11.4 ml, 180 mmol), and a molar solution of diethylaluminum chloride in hexane (164 ml, 164 mmol) is added drop-wise in succession to a solution of 3-chloro-4-methoxy-aniline (23.6 g, 150 mmol) in an inert atmosphere at 0° C. The reaction medium is heated to reflux for 1 h then cooled to 0° C., hydrolized by adding carefully 2N hydrochloric acid (90 ml), then maintained at reflux for 1 h. It is chilled again and a concentrated solution of sodium bicarbonate is added to pH 14. The solution is extracted with ethyl acetate, the organic phase is washed in water, then in salt water. Dry it on magnesuim sulfate, filter and evaporate under reduced pressure. The residue is recovered in isopentane, decanted, then recover what is insoluble in the minimum amount of isopropyl ether, and isopentane is added to precipitate the product. Filter and dry under vacuum. 17.26 g of a brown solid are obtained.

1. customThis product is obtained
2. temperatureThe reaction medium is heated
3. temperatureto reflux for 1 h
4. temperaturemaintained
5. temperatureat reflux for 1 h
6. temperatureIt is chilled again
7. extractionThe solution is extracted with ethyl acetate
8. washthe organic phase is washed in water
9. dry with materialDry it on magnesuim sulfate
10. filtrationfilter
11. customevaporate under reduced pressure
12. customThe residue is recovered in isopentane
13. customdecanted
14. customrecover what
15. additionis added
16. customto precipitate the product
17. filtrationFilter
18. customdry under vacuum