HRID1448518
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 0.70 g. (3.02 mmoles) of 2-methyl-9-methoxy-2,3-dihydro-7H-furo[3,2-g][1]benzopyran-7-one in 15 ml. of diphenyl ether was added 0.70 g. of 10% Pd/C. The mixture was heated under reflux for 6.0 hours, cooled, and filtered over Celite (washing with methanol). The methanol was removed from the filtrate by rotary evaporation, and the remaining solution of the product in diphenyl ether was diluted with 200 ml. of pet. ether. After standing overnight, the solid which separated was filtered off and washed with pet. ether to yield 9-methoxy-2-methyl-7H-furo[3,2-g][1]benzopyran-7-one. Recrystallization from ethanol afforded an analytical sample, mp 149°-150°.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureunder reflux for 6.0 hours
- temperaturecooled
- filtrationfiltered over Celite (washing with methanol)
- customThe methanol was removed from the filtrate by rotary evaporation
- additionthe remaining solution of the product in diphenyl ether was diluted with 200 ml
- customthe solid which separated
- filtrationwas filtered off
- washwashed with pet. ether