反応 #2199220

反応方程式

Bromacetyl chloride

N-hexylbenzylamine

triethylamine

→

desired product

収率 58.4%

N-benzyl-2-bromo-N-hexylacetamide

収率 58.4%

溶媒

DCM

DCM

反応条件

後処理

1. 1
   温度cooled in an ice-bath
2. 2
   その他was allowed going up to room temperature
3. 3
   洗浄The mixture was washed with water
4. 4
   workup.ADDITIONmixed with 1% hydrochloric acid (water phase pH˜4-5) and brine
5. 5
   乾燥dried with magnesium sulphate
6. 6
   その他evaporated

実験手順

N-hexylbenzylamine (4.2 g, 21.953 mmol) and triethylamine (3.98 ml, 28.539 mmol) were mixed in DCM (20 ml) and cooled in an ice-bath. Bromacetyl chloride (3.455 mg, 21.953 mmol) in DCM (5 ml) was added. The mixture was stirred over weekend and the temperature was allowed going up to room temperature. The mixture was washed with water mixed with 1% hydrochloric acid (water phase pH˜4-5) and brine, dried with magnesium sulphate, and evaporated. Column chromatography of the residue on silica gel using ethyl acetate/heptane (10:90, then 20:80) as eluant gave 4.0 g desired product, yield 58%.

出典