HRID51289

反应详情

EQUATION

反应方程式

HRID 51289 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1,3,3-trimethylbicyclo[2.2.1]hept-2-ylamine (5 g, 26.3 mmol) in methylene chloride (20 ml) and triethylamine (4 ml) was added chloroacetyl chloride (2.1 ml, 26.4 mmol) dropwise. The resulting solution was stirred for 12 hours, then the solvent removed under reduced pressure. The residue was partitioned between ethyl acetate and water, the organic layer washed with brine, and dried over magnesium sulfate. The ethyl acetate solution was absorbed onto silica gel, which was eluted with 10% ethyl acetate/hexane, to yield 2-chloro-N-(1,3,3-trimethylbicyclo[2,2,1]hept-2-yl)acetamide as a white solid.

WORKUP

后处理

  1. customthe solvent removed under reduced pressure
  2. customThe residue was partitioned between ethyl acetate and water
  3. washthe organic layer washed with brine
  4. dry with materialdried over magnesium sulfate
  5. customThe ethyl acetate solution was absorbed onto silica gel, which
  6. washwas eluted with 10% ethyl acetate/hexane