반응 #993338

반응 방정식

(R)-methyl 5-(sec-butylamino)-4-(aminocarbonyl)-2-methylbenzoate

sodium hydroxide

→

(R)-5-(sec-butylamino)-4-(aminocarbonyl)-2-methylbenzoic acid

수율 74.2%

용매

methanol

dichloromethane

반응 조건

후처리

1. 1
   온도was cooled to room temperature
2. 2
   기타all volatiles were removed by rotary evaporation
3. 3
   여과The yellow precipitate was collected by filtration
4. 4
   세척washed with water

실험 절차

To a solution of (R)-methyl 5-(sec-butylamino)-4-(aminocarbonyl)-2-methylbenzoate (300 mg, 1.13 mmol) in methanol (2.0 mL) and dichloromethane (1.0 mL) was added 2.0M aqueous sodium hydroxide solution (2.0 mL, 4.0 mmol). The reaction mixture was heated to 45° C. and stirred for 2 h, at which time it was cooled to room temperature and all volatiles were removed by rotary evaporation. To the residual solution was slowly added 1.0M aqueous hydrochloric acid until pH<2. The yellow precipitate was collected by filtration and washed with water to afford (R)-5-(sec-butylamino)-4-(aminocarbonyl)-2-methylbenzoic acid (210 mg, 65%). MS (EI) for C13H18N2O3: 251 (MH+).

출처