HRID1858091

反应详情

EQUATION

反应方程式

HRID 1858091 的结构方程式

PROCEDURE

实验过程

To a solution of 2-(2-hydroxyethyl)-piperidine-1-carboxylic acid tert-butyl ester (10 g in 450 mL dry tetrahydrofuran) was added 22.3 g of 7-chloro-3-(3,5-dimethylphenyl)-4-hydroxy-6-iodo-1H-quinolin-2-one followed by 13.7 g of triphenylphosphine and the mixture stirred at room temperature. To this was added 8.2 mL of diethyl azodicarboxylate (DEAD) and stirring was continued for 72 hours. At this time the solvents were removed to a minimum volume in vacuo and the mixture filterd through a silica gel pad to remove the phosphine by-products. The filtrate was concentrated in vacuo to provide the partially purified title compound (17.5 g).

WORKUP

后处理

  1. stirringstirring
  2. customAt this time the solvents were removed to a minimum volume in vacuo
  3. customthe mixture filterd through a silica gel pad to remove the phosphine by-products
  4. concentrationThe filtrate was concentrated in vacuo
  5. customto provide the
  6. custompartially purified title compound (17.5 g)