HRID1756333

反应详情

EQUATION

反应方程式

HRID 1756333 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under the conditions of example 1B, 652 mg of 2-bromo-6-[(1E)-(3RS)-3-hydroxy-1-undecenyl]-pyridine in 3 ml of tetrahydrofuran is mixed with 2.75 ml of n-butyllithium (1.6 molar in hexane) and 427 mg of isophthalic acid dimethyl ester in 3 ml of tetrahydrofuran, worked up and chromatographed on silica gel with hexane/ethyl acetate=95/5 to 75/25. 130 mg of an oily crude product is obtained, which is subjected to complete purification of the high-pressure liquid chromatography on silanized silica gel (RP18 material) with methanol/H2O=85/15. 58 mg of the title compound is thus obtained as colorless oil.

WORKUP

后处理

  1. customchromatographed on silica gel with hexane/ethyl acetate=95/5 to 75/25