HRID397433

反应详情

EQUATION

反应方程式

HRID 397433 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. concentrationThe reaction was concentrated
  2. filtrationThe precipitate was filtered
  3. washwashed with water
  4. filtrationfiltered
  5. customdried