反応 #470810

反応方程式

3-aminobenzyl alcohol

ethyl chloroformate

potassium carbonate

→

Ethyl(3-hydroxymethylphenyl)carbamate

溶媒

dichloromethane

反応条件

後処理

1. 1
   温度subsequently cooled to 0° C
2. 2
   workup.ADDITIONAfter the addition
3. 3
   workup.STIRRINGthe reaction mixture is stirred for 20 h and at the same time
4. 4
   温度slowly warmed to room temperature
5. 5
   その他formed (evolution of gas!)
6. 6
   その他The organic phase is separated off
7. 7
   抽出the aqueous phase is extracted with 200 ml of dichloromethane
8. 8
   洗浄the combined organic phases are washed with saturated sodium chloride solution
9. 9
   乾燥dried over sodium sulfate
10. 10
    その他the solvent is removed by distillation

実験手順

50 g (406 mmol) of 3-aminobenzyl alcohol are suspended in 750 ml of dichloromethane under a nitrogen atmosphere, the mixture is stirred at room temperature for 30 min and subsequently cooled to 0° C. 49 g (452 mmol) of ethyl chloroformate are slowly added dropwise. After the addition, the reaction mixture is stirred for 20 h and at the same time slowly warmed to room temperature. 300 ml of 1M potassium carbonate solution are added to the suspension formed (evolution of gas!). The organic phase is separated off, the aqueous phase is extracted with 200 ml of dichloromethane, the combined organic phases are washed with saturated sodium chloride solution, dried over sodium sulfate, and the solvent is removed by distillation.

出典