HRID2196553

反应详情

EQUATION

反应方程式

HRID 2196553 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 112 (361 mg, 0.796 mmol) in EtOH (3.2 mL) was added (2-Methoxy-benzyl)-hydrazine (242 mg, 1.592 mmol) and the resulting solution was allowed to stir for 1 h at room temperature, and for 2 h at 75° C. The solvent was evaporated, saturated NaHCO3 was added and the mixture extracted with EtOAc. After the usual work-up the residue was purified via Biotage (10% to 60% EtOAc/Hexane; 12M column) to afford 113 (81 mg. 18.3% yield) as white solid. LRMS (ESI): calc. 555.6; found 556.3 (MH)+.

WORKUP

后处理

  1. waitfor 2 h at 75° C
  2. customThe solvent was evaporated
  3. additionsaturated NaHCO3 was added
  4. extractionthe mixture extracted with EtOAc
  5. customAfter the usual work-up the residue was purified via Biotage (10% to 60% EtOAc/Hexane; 12M column)