反应 #550895

ord-07f188c3a60a4c5c8c1a101bdc5fd9fe

反应方程式

COC(=O)C1CN=C(Cc2ccc(OC)c(OC)c2)c2cc(OC)c(OC)cc21.Cl
3,4-dihydro-6,7-dimethoxy-1-[(3,4-dimethoxyphenyl)methyl]-4-isoquinoline carboxylic acid methyl ester, hydrochloride
C1CCC2CCCCC2C1
decalin
Cl
hydrochloric acid
COC(=O)c1cnc(Cc2ccc(OC)c(OC)c2)c2cc(OC)c(OC)cc12
6,7-dimethoxy-1-[(3,4-dimethoxyphenyl)methyl]-4-isoquinolinecarboxylic acid methyl ester
收率 115.3%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度refluxed for 2 hours
  2. 2
    其他the catalyst was removed by filtration
  3. 3
    洗涤The aqueous solution was washed with ether
  4. 4
    萃取the product was extracted with ethyl acetate
  5. 5
    其他dried
  6. 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°.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04544657uspto-grants-1985_10