反应详情

To a suspension of 1-methyl-4-phenoxycarbonylamino-5-triphenylmethylaminopyrazole (253.6 g) in N,N-dimethylformamide (1.5 L) were added triethylamine (59.5 g) and tert-butyl N-(2-aminoethyl)carbamate (94.2 g) in N,N-dimethylformamide (254 ml). The mixture was stirred for 5 hours and poured into water (10.6 L). The slurry was stirred for 1 hour. The precipitated solid was collected by filtration and dried to give a crude product. The crude product was suspended in N,N-dimethylformamide, and the suspension was heated under reflux for 20 minutes. The suspension was cooled to ambient temperature over 4 hours. The solid was collected by filtration, washed with acetonitrile and dried to give 4-[N-(2-tert-butoxycarbonylaminoethyl)carbamoylamino]-1-methyl-5-triphenylmethylaminopyrazole (261.2 g).

1. stirringThe slurry was stirred for 1 hour
2. filtrationThe precipitated solid was collected by filtration
3. customdried
4. customto give a crude product
5. temperaturethe suspension was heated
6. temperatureunder reflux for 20 minutes
7. filtrationThe solid was collected by filtration
8. washwashed with acetonitrile
9. customdried