تفاعل #75468
ord-f7f961427d9648d283d0fa156689af53
معادلة التفاعل
المتفاعلات
الكواشف
ظروف التفاعل
المعالجة
- 1غسيلthe organic phase is washed twice with water
- 2تجفيفAfter drying the organic phase over sodium sulfate
- 3أخرىthe solvent is removed in a water
- 4أخرىThe obtained crude product
- 5أخرىis purified by column chromatography over silica gel (eluant: hexane/THF 1:3)
الإجراء التجريبي
A solution of 0.54 g (2.8 mmol) 1-methyl-4-trifluoromethylpyrrole-3-carboxylic acid and 0.39 g (3.1 mmol) oxalyl chloride in 20 ml methylene chloride is stirred for 2 hours at room temperature in the presence of a catalytic amount of DMF. Then the acid chloride solution is slowly added to a solution of 0.57 g (2.8 mmol) 3-amino4-(4′-chlorophenyl)pyridine, 0.34 g (3.4 mmol) triethylamine and 15 ml methylene chloride. The resulting mixture is then stirred for 16 hours at room temperature. After the addition of ethylacetate, the organic phase is washed twice with water. After drying the organic phase over sodium sulfate, the solvent is removed in a water let vacuum. The obtained crude product is purified by column chromatography over silica gel (eluant: hexane/THF 1:3). Yield: 0.4 g 1-methyl-4-trifluoromethyl-1-1-pyrrole-3-carboxylic acid [4-(4′-chlorophenyl)pyridin-3yl]amide in the form of yellowish crystals; m.p.: 178-180° C.