HRID2165275

反应详情

EQUATION

反应方程式

HRID 2165275 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

N2 -(t Butyloxycarbonyl)-N-(Phenylmethoxy)-L-threonineamide (244 g) was dissolved in 1.2 liters of pyridine and the solution was cooled to 0° C. With stirring 120 grams of methanesulfonyl chloride was added dropwise at 0°-5° C. After 2.5 hours, the reaction mixture was poured into a mixture of 1500 ml of 2N hydrochloric acid and ice and concentrated HCl was added to adjust the pH of the mixture to 4. The title compound crystallized, and, after stirring for 1 hour, was filtered off, washed with water and petroleum ether. After drying at room temperature the yield was 356.4 grams, which contained a considerable amount of water, melting point 128°-130° C. dec.

WORKUP

后处理

  1. additionwas added dropwise at 0°-5° C
  2. additionwas added
  3. customThe title compound crystallized
  4. filtrationwas filtered off
  5. washwashed with water and petroleum ether
  6. customAfter drying at room temperature the yield was 356.4 grams, which