HRID1706599
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
2.7 parts of methylaminoacetonitrile hydrochloride was added to a solution of 2 parts of sodium hydroxide in 25 parts of water at ~15°. When the addition was complete a solution of 5.8 parts of 2-phenoxybenzoyl chloride in 50 parts of methylene chloride was added dropwise. The mixture was stirred vigorously for 5 hrs. at ~20°. The methylene chloride layer was then separated, washed with water and dried over magnesium sulfate. Removal of the magnesium sulfate by filtration and concentration of the filtrate gave 4.6 parts of N-cyanomethyl-N-methyl-2-phenoxybenzamide as a viscous oil. NMR (CDCl3) 3δ(S,3H,CH3), 4.1δ,4.3δ (2S,2H,CH2), 7.05δ, (m,9H,Aromatic H).
WORKUP
后处理
- additionWhen the addition
- additionwas added dropwise
- customat ~20°
- customThe methylene chloride layer was then separated
- washwashed with water
- dry with materialdried over magnesium sulfate
- customRemoval of the magnesium sulfate
- filtrationby filtration and concentration of the filtrate