反応 #172012

反応方程式

water

2,4,6-trifluorobenzonitrile

D-leucine amide hydrochloride

DIEA

→

(R)-2-(4-cyano-3,5-difluorophenylamino)-4-methylpentanamide

収率 26.1%

溶媒

EtOAc

DMSO

DMSO

反応条件

後処理

1. 1
   その他The organic phase was separated
2. 2
   洗浄washed with water
3. 3
   乾燥dried over Na2SO4
4. 4
   濃縮concentrated in vacuo
5. 5
   その他The residue was purified by a silica gel column
6. 6
   洗浄eluted with 20-80% EtOAc in hexane

実験手順

To a solution of 2,4,6-trifluorobenzonitrile (208 mg, 1.32 mmol) in DMSO (2 mL), a solution of D-leucine amide hydrochloride (220 mg, 1.32 mmol) and DIEA (0.688 mL, 3.96 mmol) in DMSO (5 mL) was added. After being stirred at room temperature 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 20-80% EtOAc in hexane to give (R)-2-(4-cyano-3,5-difluorophenylamino)-4-methylpentanamide (92 mg).

出典