反应详情

温度

60 °C

A solution of 3-(2-cyanopropan-2-yl)benzoic acid 3 (436 mg, 2.304 mmol), HATU (1.051 g, 2.76 mmol) and DIPEA (0.762 mL, 4.61 mmol) in DMF (9 mL) was stirred 15 min at rt. 4-bromo-3-nitroaniline (200 mg, 0.922 mmol) was added and stirred overnight at 60° C. The reaction mixture was cooled to rt and extracted with CH2Cl2. Organic layer was washed (3×) with water, dried and evaporated. Purification by chromatography heptane:EtOAc (1:1) gave N-(4-bromo-3-nitrophenyl)-3-(2-cyanopropan-2-yl)benzamide 61 (894 mg, 89%). (m/z)=388 and 390 (M+H)+.

1. temperatureThe reaction mixture was cooled to rt
2. extractionextracted with CH2Cl2
3. washOrganic layer was washed (3×) with water
4. customdried
5. customevaporated
6. customPurification by chromatography heptane:EtOAc (1:1)