HRID1691547

反应详情

EQUATION

反应方程式

HRID 1691547 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

To a solution of compound 141-B (6.55 g; 29.4 mmol) in methanol (100 mL) was added 1N NaOH (44.2 mL; 44.2 mmol) and the reaction was heated at 65° C. for 18 h. The reaction was cooled, the solvent evaporated under reduced pressure, the residue dissolved in H2O, cooled to 0° C., acidified with 2N HCl, and the solid filtered, washed with H2O, and dried in vacuo to afford compound 141-C as a white solid (6.01 g, 98%). 1H-NMR (DMSO-d6): δ 3.84 (s, 3H), 7.05-7.08 (m, 1H), 7.60-7.61 (d, 1H), 7.87-7.89 (d, 1H), 8.01 (s, 1H), 13.24 (s, 1H); MS: m/z 208.9 (MH+).

WORKUP

后处理

  1. temperatureThe reaction was cooled
  2. customthe solvent evaporated under reduced pressure
  3. dissolutionthe residue dissolved in H2O
  4. temperaturecooled to 0° C.
  5. filtrationthe solid filtered
  6. washwashed with H2O
  7. customdried in vacuo