HRID1818153

反应详情

EQUATION

反应方程式

HRID 1818153 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under a nitrogen atmosphere, a solution of tert-butyl N-(4-aminobutyl)carbamate (13.8 g, 73.4 mmol) and triethylamine (15.3 mL, 110 mmol) was cooled to 0° C. Methanesulfonyl chloride (6.3 mL, 81 mmol) was added, and the reaction was allowed to warm to ambient temperature and stirred overnight. Aqueous acetic acid (200 mL of 10%) was added. The organic layer was then separated and washed with water (200 mL), saturated aqueous sodium bicarbonate (200 mL), water (200 mL), and brine; dried over sodium sulfate; filtered; and concentrated under reduced pressure to provide 18.9 g of tert-butyl [4-(methanesulfonylamino)butyl]carbamate as an off-white solid.

WORKUP

后处理

  1. customThe organic layer was then separated
  2. washwashed with water (200 mL), saturated aqueous sodium bicarbonate (200 mL), water (200 mL), and brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationand concentrated under reduced pressure