반응 #172015

반응 방정식

2-bromo-4,5-difluorobenzonitrile

D-leucine amide hydrochloride

DIEA

Water

→

(R)-2-(5-bromo-4-cyano-2-fluorophenylamino)-4-methylpentanamide

수율 53.3%

용매

DMSO

EtOAc

반응 조건

후처리

1. 1
   기타The organic phase was separated
2. 2
   세척washed with water
3. 3
   건조dried over Na2SO4
4. 4
   농축concentrated in vacuo
5. 5
   기타The residue was purified by a silica gel column
6. 6
   세척eluted with 0-50% EtOAc in hexane

실험 절차

A solution of 2-bromo-4,5-difluorobenzonitrile (218 mg, 1.00 mmol), D-leucine amide hydrochloride (185 mg, 1.10 mmol) and DIEA (0.600 mL, 3.45 mmol) in DMSO (3 mL) was stirred at 120 C for 18 h. Water and EtOAc were added. The organic phase was separated, washed with water, dried over Na2SO4, concentrated in vacuo. The residue was purified by a silica gel column, eluted with 0-50% EtOAc in hexane to give (R)-2-(5-bromo-4-cyano-2-fluorophenylamino)-4-methylpentanamide (175 mg).

출처