تفاعل #60244

معادلة التفاعل

7-Fluoro-6-(4-bromo-2-methyl-phenylamino)-1H-benzoimidazole-5-carboxylic acid methyl ester

NaOH

HCl

→

desired product

المردود 95.4%

7-Fluoro-6-(4-bromo-2-methyl-phenylamino)-1H-benzoimidazole-5-carboxylic acid

المردود 95.4%

المذيبات

MeOH

ethyl acetate

water

ظروف التفاعل

المعالجة

1. 1
   أخرىthe layers separated
2. 2
   غسيلThe organic layer is washed with brine
3. 3
   تجفيفdried (Na2SO4)
4. 4
   تركيزconcentrated under reduced pressure

الإجراء التجريبي

7-Fluoro-6-(4-bromo-2-methyl-phenylamino)-1H-benzoimidazole-5-carboxylic acid methyl ester 8a (63 mg, 0.167 mmol) is suspended in MeOH (1.5 mL) and 20% NaOH (400 μl) is added. After 16 hours, the reaction mixture is cooled to 0° C. and 1 N HCl solution is added dropwise until pH is 2 to 3. The reaction mixture is diluted with ethyl acetate and water and the layers separated. The organic layer is washed with brine, dried (Na2SO4) and concentrated under reduced pressure to give 58 mg (95%) of desired product: MS APCI (+) m/z 366, 364 (M+1 Br pattern) detected; MS APCI (−) m/z 364, 362 (M−1 Br pattern) detected.

المصدر