反应详情

温度

140 °C

10-chloro-6-methyl-2-propan-2-yl-2,6,9,11-tetrazabicyclo[5.4.0]undeca-7,9,11-trien-5-one (Intermediate 76, 100 mg, 0.39 mmol) and 4-amino-3-chloro-N-(1-methyl-4-piperidyl)benzamide (Intermediate 79; 127 mg, 0.47 mmol) were suspended in 4-methyl-2-pentanol (3 mL) and p-toluenesulphonic acid monohydrate (74 mg, 0.97 mmol) added. The mixture was heated at 140° C. for 4 hours The mixture was cooled causing a white solid to formed. The whole mixture was diluted with MeOH to give a solution which was absorbed on to an SCX-3 column, washed with methanol and eluted with ammonia/methanol. Concentration and column chromatography (1-2-3-5% NH3 in MeOH/DCM) of the product containing fractions gave the title compound as a white solid (58 mg, 31%).

1. temperaturewas cooled
2. customto formed
3. customto give a solution which
4. customwas absorbed on to an SCX-3 column
5. washwashed with methanol
6. washeluted with ammonia/methanol
7. concentrationConcentration and column chromatography (1-2-3-5% NH3 in MeOH/DCM) of the product
8. additioncontaining fractions