反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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. B. Preparation of a Compound of Formula (1) in which R1 is Cyclohexyl and R2 is Phenyl
WORKUP
后处理
- customthe solvent removed under reduced pressure
- customThe residue was partitioned between ethyl acetate and water
- washthe organic layer washed with brine
- dry with materialdried over magnesium sulfate
- customThe ethyl acetate solution was absorbed onto silica gel, which
- washwas eluted with 10% ethyl acetate/hexane