反応 #5168

反応方程式

sodium chloride

triethylamine

(2S, 4R)-1-(t-butoxycarbonyl)-2-methylcarbamoyl-4-hydroxypyrrolidine

methanesulfonyl chloride

→

title compound

(2S, 4R)-1-(t-Butoxycarbonyl)-4-methanesulfonyloxy-2-methylcarbamoylpyrrolidine

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   workup.WAITat 15° C. for 30 minutes
2. 2
   抽出extracted with ethyl acetate
3. 3
   洗浄The extract was washed with an aqueous solution of sodium chloride
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   その他The solvent was then removed by distillation under reduced pressure

実験手順

7.11 ml of triethylamine were added, whilst ice-cooling, to a solution of 11.29 g of (2S, 4R)-1-(t-butoxycarbonyl)-2-methylcarbamoyl-4-hydroxypyrrolidine [prepared as described in step (1) above] dissolved in 120 ml of dry tetrahydrofuran, and then 3.93 ml of methanesulfonyl chloride were added to the resulting mixture, and the mixture was stirred at 0° to 5° C. for 30 minutes and then at 15° C. for 30 minutes. It was then poured into an aqueous solution of sodium chloride and extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The solvent was then removed by distillation under reduced pressure, giving 11.58 g of the title compound as colorless crystals.

出典