HRID1638988

反应详情

EQUATION

反应方程式

HRID 1638988 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a nitrogen gas flow, 562 mg of L-cysteine hydrochloride monohydrate is dissolved in an aqueous solution of 2N sodium hydroxide. To the resulting solution, 5 ml of a tetrohydrofuran solution containing 1.2 g of 2-(1-benzyloxycarbonyl-4-piperidyl)ethyl iodide is added, and stirred for 1.5 hours at room temperature. Then, 3 ml of ethanol is further added, and stirred for 2 hours. The reaction solvent is distilled off under reduced pressure. To the residue, water and ether are added, and the mixture is shaken. The water layer is separated and adjusted to pH 5 with 2N aqueous hydrochloric acid to precipitate crystals. The crystals are recrystallized from methanol to give 0.8 g of S-[2-(1-benzyloxycarbonyl-4-piperidyl)ethyl]-L-cysteine having a melting point of 185° to 188° C.

WORKUP

后处理

  1. additionis added
  2. stirringstirred for 2 hours
  3. distillationThe reaction solvent is distilled off under reduced pressure
  4. additionTo the residue, water and ether are added
  5. stirringthe mixture is shaken
  6. customThe water layer is separated
  7. customto precipitate crystals
  8. customThe crystals are recrystallized from methanol