反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 4-(3-chloro-4-fluoro-phenylamino)-5,7-dihydro-pyrrolo[2,3-d]pyrimidin-6-one (70 mg, 0.25 mmol), (5-formyl-2,4-dimethyl-1H-pyrrol-3-yl)-acetic acid (54.3 mg, 0.3 mmol) and piperidine (3 drops) in ethanol (2 mL) was stirred at room temperature for 1 day. The reaction was concentrated, the residue was suspended in 1N HCl. The precipitate was filtered, washed with water, suspended in hot ethyl acetate, filtered and dried to give 42 mg (38%) of the title compound. 1H NMR (300 MHz, DMSO-d6) δ 13.21 (br s, 1H, NH), 12.17 (br s, 1H, COOH), 11.65 (s, 1H, NH), 9.13 (s, 1H), 8.26 (s, 1H), 7.71 (m, 1H), 7.3-7.4 (m, 3H), 3.37 (s, 2H, CH2), 2.3 (s, 3H, CH3), 2.10 (s, 3H, CH3). MS 442 [M++1].
WORKUP
后处理
- concentrationThe reaction was concentrated
- filtrationThe precipitate was filtered
- washwashed with water
- filtrationfiltered
- customdried