反应详情

To a solution of 4-chloro-5,6,7,8-tetrahydrobenzo[1,2-b]pyrimidino[5,4-d]selenophene (700 mg, 2.57 mmol, from step b of example 1) in DMF (10 mL) was added sequentially 5-tert-butyl-3-aminothiophene-2-carboxamide (700 mg, 3.6 mmol) and powdered NaOH (310 mg, 7.7 mmol) at rt. Work-up of the mixture as described in example 2, gave the product as a yellow color solid, mp 240-244° C. 1H NMR (400 MHz, DMSO-d6): δ 11.38 (1H, s, exchangeable with D2O), 8.45 (1H, s), 8.27 (1H, s), 7.53 (2H, s, exchangeable with D2O), 3.15 (2H, br s), 2.90 (2H, br s), 1.84-1.85 (4H, m), 1.39 (9H, s); 13C NMR (100 MHz, DMSO-d6): δ 170.9, 166.1, 158.0, 153.1, 151.4, 143.4, 138.2, 128.2, 119.5, 119.2, 109.2, 34.5, 31.7, 27.7, 27.4, 22.4, 22.1; LC-MS (positive ion mode): m/z 433, 435 (M+H)+.

1. customgave the product as a yellow color solid, mp 240-244° C