反応 #171999

反応方程式

(R)-2-(3-bromo-4-cyanophenylamino)-3-phenylpropanamide

5-amino-3-methylisothiazole hydrochloride

BINAP

K2CO3

→

(R)-2-(4-cyano-3-(3-methylisothiazol-5-ylamino)phenylamino)-3-phenylpropanamide

溶媒

dioxane

反応条件

後処理

1. 1
   その他was degassed with Ar
2. 2
   workup.ADDITIONWater and EtOAc were added
3. 3
   ろ過After being filtered
4. 4
   その他the organic phase was separated
5. 5
   洗浄washed with 1N HCl
6. 6
   乾燥dried over Na2SO4
7. 7
   濃縮concentrated in vacuo

実験手順

A mixture of (R)-2-(3-bromo-4-cyanophenylamino)-3-phenylpropanamide (102 mg, 0.296 mmol), 5-amino-3-methylisothiazole hydrochloride (58 mg, 0.385 mmol), BINAP (25 mg, 0.040 mmol), Pd(OAc)2 (20 mg, 0.089 mmol) and K2CO3 (150 mg, 1.08 mmol) in dioxane (3 mL) was degassed with Ar, then was stirred at 120 C for 18 h. Water and EtOAc were added. After being filtered, the organic phase was separated, washed with 1N HCl, dried over Na2SO4, concentrated in vacuo to give (R)-2-(4-cyano-3-(3-methylisothiazol-5-ylamino)phenylamino)-3-phenylpropanamide as a crude residue.

出典