反応 #721989

反応方程式

4,4′-methylenedianiline

potassium carbonate

Benzyl chloroformate

→

4-(4-aminobenzyl)phenyl-carbamic acid benzyl ester

溶媒

ethyl acetate

water

反応条件

後処理

1. 1
   workup.STIRRINGThe resulting mixture was stirred for 1 hour
2. 2
   その他the organic layer was separated
3. 3
   抽出the aqueous layer extracted with additional ethyl acetate
4. 4
   洗浄The combined organic extracts were washed with water and brine
5. 5
   乾燥dried (Na2SO4)
6. 6
   その他the solvent removed in vacuo
7. 7
   その他The crude mixture was isolated by column chromatography on silica gel
8. 8
   洗浄eluting with 30% ethyl acetate/hexanes

実験手順

A mixture of 4,4′-methylenedianiline (19.8 g), potassium carbonate (20 g) in ethyl acetate (300 mL) and water (200 mL) was stirred in an ice bath. Benzyl chloroformate (15 mL) was slowly added to the mixture. The resulting mixture was stirred for 1 hour, then the organic layer was separated, and the aqueous layer extracted with additional ethyl acetate. The combined organic extracts were washed with water and brine, dried (Na2SO4), and the solvent removed in vacuo. The crude mixture was isolated by column chromatography on silica gel, eluting with 30% ethyl acetate/hexanes, to give 4-(4-aminobenzyl)phenyl-carbamic acid benzyl ester as solid.

出典