HRID378975

反应详情

EQUATION

反应方程式

HRID 378975 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of vanillin (12.49 g, 82.1 mmoles) in dimethylformamide was added with Na2CO3 (17.4 g, 164 mmoles) and KI (catalytic amount). The mixture was brought to 90° C. then slowly added with methansulfonic acid 5-phenyl-pentyl ester (24.87 g, 103 mmoles) obtained as described in example 11, in dimethylformamide (40 ml). After 1.5 hours the mixture was poured into 1N HCl and thrice extracted with pentane, anhydrified and dried. The residue was purified by silica gel flash chromatography (eluent: petrolatum/ethyl acetate 9:1), so 7.46 g of the title product were obtained (yield: 97%).

WORKUP

后处理

  1. customwas brought to 90° C.
  2. customobtained
  3. extractionextracted with pentane
  4. customdried
  5. customThe residue was purified by silica gel flash chromatography (eluent: petrolatum/ethyl acetate 9:1)