HRID13526

反应详情

EQUATION

反应方程式

HRID 13526 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 50 mL round bottom flask was charged with 1 (680 mg, 2.5 mmol), hydroxylamine HCl (191 mg, 2.75 mmol), pyridine (0.25 mL, 3.0 mmol) and ethanol (10 mL). The resulting reaction mixture was stirred at rt overnight. The crude product was concentrated, absorbed onto silica gel, and purified by flash chromatography (97:3 CH2Cl2/MeOH to give 2 as an orange solid. LCMS m/z 289.2 (MH+), tR=2.06 min.

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. concentrationThe crude product was concentrated
  3. customabsorbed onto silica gel
  4. custompurified by flash chromatography (97:3 CH2Cl2/MeOH