تفاعل #60312

معادلة التفاعل

4,5-Diamino-3-chloro-2-phenylamino-benzoic acid methyl ester

formamidine acetate

→

clean desired product

المردود 100.3%

7-Chloro-6-phenylamino-3H-benzoimidazole-5-carboxylic acid methyl ester

المردود 100.3%

المذيبات

EtOAc

EtOH

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe reaction mixture is cooled to room temperature
2. 2
   غسيلwashed with water (3×), saturated NaHCO3, and brine
3. 3
   تجفيفThe combined organic extracts are dried (Na2SO4)
4. 4
   تركيزconcentrated under reduced pressure

الإجراء التجريبي

4,5-Diamino-3-chloro-2-phenylamino-benzoic acid methyl ester 6b (0.32 g, 1.09 mmol) and formamidine acetate (72 mg, 1.64 mmol) in EtOH (36 mL) are heated, with stirring, to 80° C. After 44 hours, the reaction mixture is cooled to room temperature and diluted with EtOAc and washed with water (3×), saturated NaHCO3, and brine. The combined organic extracts are dried (Na2SO4) and concentrated under reduced pressure to give 0.33 g (99%) clean desired product as a solid. MS APCI (+) m/z 302.3 (M+1) detected.

المصدر