反応 #81391

反応方程式

valinol

triethylamine

benzyl chloroformate

→

N-benzyloxycarbonyl-valinol

収率 95.6%

溶媒

methylene chloride

methylene chloride

反応条件

後処理

1. 1
   洗浄washed with 1N HCl (2×), brine
2. 2
   乾燥dried with anhydrous magnesium sulfate
3. 3
   ろ過The resulting mixture was filtered
4. 4
   その他evaporated

実験手順

To a stirred solution of valinol (13.96 g, 0.14 mol) and triethylamine (18.87 mL, 0.14 mol) in 250 mL of dry methylene chloride cooled to 0° C. under a nitrogen atmosphere was added 19.3 mL (0.14 mol) of benzyl chloroformate dropwise over 20 min. After warming to RT overnight, the mixture was diluted with methylene chloride (100 mL) and washed with 1N HCl (2×), brine and dried with anhydrous magnesium sulfate. The resulting mixture was filtered and evaporated to give 30.70 g (95.6%) of N-benzyloxycarbonyl-valinol as a white solid: Rf =0.27 (silica gel; 1:1 hexane:ethyl acetate). Used without further purification.

出典