HRID1406094

反应详情

EQUATION

反应方程式

HRID 1406094 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-hydroxy-7-phenylsulfanyl-isoquinoline-3-carboxylic acid butyl ester (0.20 g) and L-alanine (0.75 g) in 0.5 M NaOMe/MeOH (11.3 ml) was heated to reflux for 36 h. After coolng, reaction mixture was concentrated. The residue was suspended in water (50 ml) and extracted with ethyl acetate (50 ml) which was discarded. The aqueous layer was acidified by 2 N HCl aqueous solution. Extracted with ethyl acetate (2×50 ml). Combined organic layers were dried over magnesium sulfate, filtered, and concentrated to give the title compound (0.15 g). MS-(−)-ion: M−1=367.1.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 36 h
  3. customreaction mixture
  4. concentrationwas concentrated
  5. extractionextracted with ethyl acetate (50 ml) which
  6. extractionExtracted with ethyl acetate (2×50 ml)
  7. dry with materialCombined organic layers were dried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated