反应 #1483108

反应方程式

2-bromo-2-methylpropionyl bromide

tridecan-2-ol

2-tridecanol

triethylamine

→

98

收率 97.6%

tridecen-2-yl 2-bromopropanoate

收率 97.6%

溶剂

toluene

反应条件

后处理

1. 1
   其他The reaction mixture was quenched with saturated sodium bicarbonate solution
2. 2
   workup.STIRRINGstirred for 15 minutes at 25-35° C
3. 3
   其他The aqueous and organic layers were separated
4. 4
   洗涤The organic layer was washed with brine
5. 5
   洗涤the combined organic layers were washed with brine solution
6. 6
   干燥The organic layer was dried over Na2SO4
7. 7
   浓缩concentrated under vacuum

实验过程

To a stirred solution of tridecan-2-ol 68 (5 g, 24.9 mmol) in toluene (50 mL) was added triethylamine (3.5 mL, 27.45 mmol)) and followed by 2-bromo-2-methylpropionyl bromide 97 (6.31 g, 27.45 mmol) at 5-10° C. The reaction mixture was stirred for 3 hour at 55-60° C., and the reaction was monitored by TLC. The reaction mixture was quenched with saturated sodium bicarbonate solution and stirred for 15 minutes at 25-35° C. The aqueous and organic layers were separated. The organic layer was washed with brine, and the combined organic layers were washed with brine solution. The organic layer was dried over Na2SO4 and concentrated under vacuum to afford crude 98 (8.1 g, yield: 96%) as a liquid.

来源