HRID2249426

反应详情

EQUATION

反应方程式

HRID 2249426 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

5-Acetyl-1-benzofuran (536 mg, 3.35 mmol) and diethyl ketomalonate (642 mg, 3.69 mmol) were mixed together, and the mixture was stirred for 34 hours at 120° C. Hydrazine monohydrate (247 mg, 4.93 mmol) was added to a solution of the reaction mixture in isopropanol (8.5 mL), and the resultant mixture was heated with stirring for six hours at 100° C. A 2-mol/L aqueous sodium hydroxide solution (5.2 mL) was added thereto, and the mixture was further stirred for four hours at 100° C. The mixture was cooled with ice, and concentrated hydrochloric acid was added thereto, to thereby acidify the heated system. The formed precipitates were collected through filtration, thoroughly washed with water, and dried, to thereby yield 397 mg of the title compound as a yellow powder (46.2%).

WORKUP

后处理

  1. stirringwith stirring for six hours at 100° C
  2. stirringthe mixture was further stirred for four hours at 100° C
  3. additionwas added
  4. customThe formed precipitates
  5. filtrationwere collected through filtration
  6. washthoroughly washed with water
  7. customdried