Bromoacetyl bromide → Acetamide, 2-bromo-N-methyl-N-2-propynyl-

温度

25 °C

A solution of 13.8 g (0.2 mol) of N-methylpropargylamine in 20 ml methylene chloride was added dropwise to a stirred and cooled (below 15°C.) solution of 40.2 g (0.2 mol) bromoacetyl bromide and 16 g (0.2 mol) sodium bicarbonate in 250 ml methylene chloride. The reaction mixture was allowed to warm to about 25°C. and stirred for 2 hours. The reaction mixture was then filtered and evaporated under reduced pressure to give an oily residue. The residue was diluted with 150 ml ether to form a two-phase mixture consisting of an ether phase and a dark oil. The ether phase was separated, dried over magnesium sulfate, and evaporated to give 32.3 g of N-methyl-N-propargyl-α-bromoacetamide.

1. stirringstirred for 2 hours
2. filtrationThe reaction mixture was then filtered
3. customevaporated under reduced pressure
4. customto give an oily residue
5. customto form a two-phase mixture
6. customThe ether phase was separated
7. dry with materialdried over magnesium sulfate
8. customevaporated

ORDレコード

ord-4e2ab9a786d7478fbf79ca559a0316c0

出典データセット

uspto-grants-1976_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US03944607