반응 #1106680

반응 방정식

hydrochloric acid

Catechol

sodium methoxide

methyl dichloroacetate

→

benzo[1,3]dioxole-2-carboxylic acid methyl ester

용매

Water

methanol

반응 조건

후처리

1. 1
   온도The solution was heated
2. 2
   온도to reflux overnight
3. 3
   추출the mixture was extracted with diethyl ether (3×100 mL)
4. 4
   건조The combined organic solution was dried with MgSO4
5. 5
   농축concentrated to a brown solid
6. 6
   기타chromatographed (2% ethyl acetate in hexane)

실험 절차

Catechol (10.26 g, 93.2 mmol), sodium methoxide (25% by weight in methanol, 40.3 g, 186 mmol), and methyl dichloroacetate (13.3 g, 93.2 mmol) were combined in dry methanol (100 mL). The solution was heated to reflux overnight. The reaction was cooled to room temperature, acidified by addition of concentrated hydrochloric acid and then reduced in volume under vacuum to about 50 mL. Water was added and the mixture was extracted with diethyl ether (3×100 mL). The combined organic solution was dried with MgSO4, concentrated to a brown solid, and chromatographed (2% ethyl acetate in hexane) to yield benzo[1,3]dioxole-2-carboxylic acid methyl ester as a colorless oil.

출처