反应 #550895
ord-07f188c3a60a4c5c8c1a101bdc5fd9fe
反应方程式
3,4-dihydro-6,7-dimethoxy-1-[(3,4-dimethoxyphenyl)methyl]-4-isoquinoline carboxylic acid methyl ester, hydrochloride
decalin
hydrochloric acid
→
6,7-dimethoxy-1-[(3,4-dimethoxyphenyl)methyl]-4-isoquinolinecarboxylic acid methyl ester
收率 115.3%
反应物
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度refluxed for 2 hours
- 2其他the catalyst was removed by filtration
- 3洗涤The aqueous solution was washed with ether
- 4萃取the product was extracted with ethyl acetate
- 5其他dried
- 6其他evaporated
实验过程
A mixture of 3.9 g of 3,4-dihydro-6,7-dimethoxy-1-[(3,4-dimethoxyphenyl)methyl]-4-isoquinoline carboxylic acid methyl ester, hydrochloride, 100 ml of decalin and 2 g of 10% palladium on carbon was stirred and refluxed for 2 hours. The cooled mixture was diluted with water, acidified with 6N hydrochloric acid, and the catalyst was removed by filtration. The aqueous solution was washed with ether, made basic with excess ammonium hydroxide, and the product was extracted with ethyl acetate, dried, and evaporated to give 4.1 g of crude 6,7-dimethoxy-1-[(3,4-dimethoxyphenyl)methyl]-4-isoquinolinecarboxylic acid methyl ester. Crystallization from ether provided the analytically pure material, mp 127°-128°.