反应详情

To a cooled (ice bath) stirred solution of 130.3 g (1.05 mole) of 2-methoxyphenol in 750 mL of carbon disulfide was continuously added 306.6 g (2.3 mole) of anhydrous aluminum chloride portionwise. The stirred, cooled mixture was then treated dropwise with 80 mL (113 g, 1.0 mole) of 2-chloroacetyl chloride. After the addition was completed, the mixture was heated at reflux temperature for 20 hr, cooled, and poured into a mixture of 2 kg of crushed ice and 200 ml of concentrated hydrochloric acid. The solid which gradually crystallized was washed with water and carbon disulfide and dried. The solid was recrystallized from isopropyl ether containing a few drops of 2-propanol to yield 128.3 g (64% yield) of the title compound, mp 102°-103° C.

1. temperatureTo a cooled (ice bath)
2. temperatureThe stirred, cooled mixture
3. additionAfter the addition
4. temperaturethe mixture was heated
5. temperatureat reflux temperature for 20 hr
6. temperaturecooled
7. customThe solid which gradually crystallized
8. washwas washed with water and carbon disulfide
9. customdried
10. customThe solid was recrystallized from isopropyl ether containing a few drops of 2-propanol