تفاعل #721989

معادلة التفاعل

4,4′-methylenedianiline

potassium carbonate

Benzyl chloroformate

→

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

المذيبات

ethyl acetate

water

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGThe resulting mixture was stirred for 1 hour
2. 2
   أخرىthe organic layer was separated
3. 3
   استخلاصthe aqueous layer extracted with additional ethyl acetate
4. 4
   غسيلThe combined organic extracts were washed with water and brine
5. 5
   تجفيفdried (Na2SO4)
6. 6
   أخرىthe solvent removed in vacuo
7. 7
   أخرىThe crude mixture was isolated by column chromatography on silica gel
8. 8
   غسيلeluting with 30% ethyl acetate/hexanes

الإجراء التجريبي

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.

المصدر