HRID1409372

反应详情

EQUATION

反应方程式

HRID 1409372 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Lithium (Z)-4-(1-benzyl-1H-imidazol-4-yl)-1-ethoxy-1,4-dioxobut-2-en-2-olate (9.80 mmol, 3.0 g) was suspended in dry ethanol (20 ml). Hydrazine dihydro-chloride (12.74 mmol, 1.337 g) was added and the resulting mixture was refluxed for 2 h. The mixture was cooled to ambient temperature and evaporated. The sticky oil was purified by trituration from ethanol. The precipitate was separated by filtration and flushed with cold ethanol. 2.614 g of the title compound was obtained. 1H-NMR (400 MHz, DMSO-d6): δ 1.31 (t, 3H), 4.33 (q, 2H), 5.81 (bs, 2H), 7.11-7.39 (m, 6H), 8.16 (bs, 1H), 9.31 (bs, 1H), 14.50 (bs, 1H).

WORKUP

后处理

  1. temperaturethe resulting mixture was refluxed for 2 h
  2. customevaporated
  3. customThe sticky oil was purified by trituration from ethanol
  4. customThe precipitate was separated by filtration
  5. customflushed with cold ethanol