反応 #1483106

反応方程式

2-bromopropionyl bromide

2-bromo propionyl bromide

2-methyltridecan-2-ol

triethylamine

→

74

収率 61.3%

2-methyltridecan-2-yl 2-bromopropanoate

収率 61.3%

溶媒

Toluene

反応条件

後処理

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

実験手順

To a stirred solution of 2-methyltridecan-2-ol 73 (5 g, 23.4 mmol) in Toluene (50 mL) was added triethylamine (3.29 mL, 23.4 mmol)) and followed by 2-bromopropionyl bromide 58 (5.11 g, 23.7 mmol) at 5-10° C. The reaction mixture was stirred for 3 hours at 55-60° C.; 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 74 (5 g, yield: 61.27%) as a liquid.

出典