HRID221406

反应详情

EQUATION

反应方程式

HRID 221406 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

Benzyl 3-(2-(tert-butyldimethylsilyloxy)-1-hydroxyethyl)phenylcarbamate (4 g) was dissolved in dry DCM (80 mL) and cooled to 0° C. under an argon atmosphere. Triethylamine (5 g) was added, followed by mesyl chloride (3.42 g) added drop-wise over a period of 2 hours. The reaction temp was maintained at 0° C. for further 2 hours. The reaction was quenched by addition of water, extracted into DCM and concentrated under vacuum at a temperature below 25° C. The crude product (3.5 g) was unstable and was used for next step as soon as possible.

WORKUP

后处理

  1. additionadded drop-wise over a period of 2 hours
  2. temperatureThe reaction temp was maintained at 0° C. for further 2 hours
  3. customThe reaction was quenched by addition of water
  4. extractionextracted into DCM
  5. concentrationconcentrated under vacuum at a temperature below 25° C