HRID1814734

反应详情

EQUATION

反应方程式

HRID 1814734 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Isobutylamino-1 -morpholin-4-yl-ethanone (1.43 g, 7.13 mmol) was dissolved in 15 mL of THF. To this solution at −78° C. was added a solution of bromoacetyl bromide (1.24 mL, 14.3 mmol) in 15 mL of THF. The mixture was warmed to room temperature and stirred for 2 h. Solvent was removed in vacuo. The residue was dissolved in 30 mL of methylene chloride, washed with saturated sodium bicarbonate, and brine, then dried over sodium sulfate. The solvent was removed in vacuo and the residue was purified by silica gel flash chromatography eluting with 2% MeOH in methylene chloride to give 2-bromo-N-isobutyl-N-(2-morpholin-4-yl-2-oxo-ethyl)-acetamide (1.37 g, 60%) as a clear oil.

WORKUP

后处理

  1. customSolvent was removed in vacuo
  2. dissolutionThe residue was dissolved in 30 mL of methylene chloride
  3. washwashed with saturated sodium bicarbonate, and brine
  4. dry with materialdried over sodium sulfate
  5. customThe solvent was removed in vacuo
  6. customthe residue was purified by silica gel flash chromatography
  7. washeluting with 2% MeOH in methylene chloride