HRID1845621

反应详情

EQUATION

反应方程式

HRID 1845621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a 100 mL round-bottomed flask was added methyl 5-chloro-4-(1,4-dimethyl-1H-pyrazol-5-yl)-2-thiophenecarboxylate (106 mg, 0.39 mmol) in Tetrahydrofuran (THF) (2 mL). 6N NaOH (2 mL, 12.00 mmol) was added slowly and the reaction mixture stirred overnight at 70° C. The reaction was cooled to room temperature, partitioned between CHCl3 and H2O and the pH of the aqueous layer was adjusted to ˜3 by the addition of 6N HCl. The layers were separated, the organic layer dried over Na2SO4 and concentrated affording the desired compound (96 mg, 0.37 mmol, 95%): LC-MS (ES) m/z=257 (M+H)+.

WORKUP

后处理

  1. temperatureThe reaction was cooled to room temperature
  2. custompartitioned between CHCl3 and H2O
  3. additionthe pH of the aqueous layer was adjusted to ˜3 by the addition of 6N HCl
  4. customThe layers were separated
  5. dry with materialthe organic layer dried over Na2SO4
  6. concentrationconcentrated