반응 #482435

반응 방정식

4-methylcatechol

NaOH

CH2Cl2

→

title intermediate

수율 71.9%

3,4-Methylenedioxytoluene

수율 71.9%

용매

ethyl acetate

반응 조건

후처리

1. 1
   온도to cool to ambient temperature
2. 2
   세척The mixture was washed with NaHCO3 (200 mL) and H2O (2×200 mL)
3. 3
   건조The organic layer was dried over Na2SO4
4. 4
   여과filtered
5. 5
   농축concentrated
6. 6
   기타to give a crude oil
7. 7
   세척Flash chromatography eluting with hexane (100%) gradient to ether/hexane (1:1)

실험 절차

A mixture of 4-methylcatechol (26.0 g, 209.4 mmol) and NaOH (18.4 g, 461.0 mmol) in CH2Cl2 (40.0 mL) was heated to 100° C. under nitrogen for 2 hours. The solution was allowed to cool to ambient temperature and diluted with ethyl acetate (500 mL). The mixture was washed with NaHCO3 (200 mL) and H2O (2×200 mL). The organic layer was dried over Na2SO4, filtered and concentrated to give a crude oil. Flash chromatography eluting with hexane (100%) gradient to ether/hexane (1:1) afforded the title intermediate as a colorless oil 20.5 g (71.9%).

출처