HRID1409382

反应详情

EQUATION

反应方程式

HRID 1409382 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 5-(cyclopropylcarbamoyl)isoxazole-3-carboxylate (1.267 mmol, 0.284 g) was dissolved in ethanol (10 ml). The mixture was cooled in an ice bath and NaOH 2 M solution (2.53 mmol, 1.267 ml) was added. The resulting mixture was stirred in cold until the reaction was complete. Ethanol was evaporated and water was added. The pH of the mixture was adjusted to 4 with HCl. The precipitate was removed by filtration. The filtrate was evaporated and purified by trituration from 1/9 MeOH/DCM. 0.058 g of the title compound was obtained. 1H-NMR (400 MHz, DMSO-d6): δ 0.57-0.66 (m, 2H), 0.67-0.75 (m, 2H), 2.77-2.88 (m, 1H), 6.97 (s, 1H), 8.85 (m, 1H).

WORKUP

后处理

  1. temperatureThe mixture was cooled in an ice bath
  2. customEthanol was evaporated
  3. additionwater was added
  4. customThe precipitate was removed by filtration
  5. customThe filtrate was evaporated
  6. custompurified by trituration from 1/9 MeOH/DCM