HRID1371860

反应详情

EQUATION

反应方程式

HRID 1371860 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine 3-(2-nitrovinyl)-6-ethoxycarbonyl-1H-indole (4.0 g, 15.37 mmol) and NaBH4 (726.7 mg, 19.21 mmol) in 100 ml of THF/Methanol (9:1) and stir at ambient temperature. After 1.5 hours, concentrate to residue. Partition the residue between brine and ethyl acetate, wash with brine, combine the organic layers, dry (Na2SO4), then evaporate to give the title compound as a yellow powder: mp 124–127° C. MS (ACPI): m/e 263.0 (M+1). Analysis for C13H14N2O4: Calcd: C, 59.54; H, 5.38; N, 10.68; found: C, 59.40; H, 5.36; N, 10.53.

WORKUP

后处理

  1. concentrationconcentrate to residue
  2. customPartition the residue between brine and ethyl acetate
  3. washwash with brine
  4. dry with materialdry (Na2SO4)
  5. customevaporate