HRID2046408

反应详情

EQUATION

反应方程式

HRID 2046408 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Methyl 5-ethenyl-4-(imidazo[1,2-b]pyridazin-3-yl)thiophene-2-carboxylate (130 mg, 0.456 mmol) was dissolved in methanol (2.28 mL) and THF (2.28 mL) and 1M KOH in MeOH (1.38 mL, 1.38 mmol) was added to the mixture. The solution was left to stir at 60° C. for 18 h. The reaction was cooled to room temperature and concentrated under reduced pressure. 1N HCl was added to the residue and the precipitate filtered. The precipitate was then dried under high vacuum affording the title compound as a yellow solid. 1H NMR (500 MHz, CD3SOCD3) δ 13.37 (s, 1H, br); 8.62 (d, 1H); 8.23 (d, 1H); 8.07 (s, 1H); 7.96 (s, 1H); 7.33 (dd, 1H); 6.91 (dd, 1H); 5.84 (d, 1H); 5.41 (d, 1H). LRMS (APCI) calc'd for (C13H9N3O2S) [M+H]+, 272.0. found 272.0.

WORKUP

后处理

  1. waitThe solution was left
  2. temperatureThe reaction was cooled to room temperature
  3. concentrationconcentrated under reduced pressure
  4. addition1N HCl was added to the residue
  5. filtrationthe precipitate filtered
  6. customThe precipitate was then dried under high vacuum