HRID659094

反应详情

EQUATION

反应方程式

HRID 659094 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 3-nitrocinnamate (1) (2.0 g, 9.04 mmol) was reduced using method A, except that SnCl2.2H2O (10.2 g, 45.20 mmol) in EtOH (20 mL) was used and after the reaction the solvent was concentrated in vacuo, Rochelle's salt and saturated NaHCO3 (1:1, 80 mL) were added, and the aqueous basified with 1N NaOH. The aqueous was extracted with EtOAc (3×40 mL), washed with Rochelle's salt/saturated NaHCO3 solution (2×40 mL), dried (MgSO4) and the solvent was concentrated in vacuo to give the title compound. Yield: 1.77 g, >100%; LC/MS tr 0.89 min; MS (ES+) m/z 192 (M+H)

WORKUP

后处理

  1. customafter the reaction the solvent
  2. concentrationwas concentrated in vacuo, Rochelle's salt and saturated NaHCO3 (1:1, 80 mL)
  3. additionwere added
  4. extractionThe aqueous was extracted with EtOAc (3×40 mL)
  5. washwashed with Rochelle's salt/saturated NaHCO3 solution (2×40 mL)
  6. dry with materialdried (MgSO4)
  7. concentrationthe solvent was concentrated in vacuo