تفاعل #157627

معادلة التفاعل

2-({[4-chloro-2-({[4-chloro-3-(trifluoromethyl)phenyl]sulfonyl}amino)phenyl]sulfanyl}methyl)benzoic acid

EDC

dimethylamine hydrochloride

→

title compound

المردود 38.0%

2-({[4-chloro-2-({[4-chloro-3-(trifluoromethyl)phenyl]sulfonyl}amino)phenyl]sulfanyl}methyl)-N,N-dimethylbenzamide

المردود 38.0%

المذيبات

CH2Cl2

water

ظروف التفاعل

المعالجة

1. 1
   استخلاصextracted with EtOAc
2. 2
   غسيلThe organic layer was washed with brine
3. 3
   تجفيفdried over Na2SO4
4. 4
   تركيزconcentrated in vacuo
5. 5
   أخرىThe residue was purified by flash column chromatography on silica gel (0˜30% EtOAc in hexane)

الإجراء التجريبي

A mixture of 2-({[4-chloro-2-({[4-chloro-3-(trifluoromethyl)phenyl]sulfonyl}amino)phenyl]sulfanyl}methyl)benzoic acid (304 mg, 0.57 mmol), DMAP (138 mg, 1.13 mmol), EDC (217 mg, 1.13 mmol), and dimethylamine hydrochloride (93 mg, 1.13 mmol) in CH2Cl2 (3 ml) was stirred at room temperature overnight. The mixture was diluted with water, extracted with EtOAc. The organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel (0˜30% EtOAc in hexane) to yield the title compound (122 mg, 38%).

المصدر