HRID1875998

反应详情

EQUATION

反应方程式

HRID 1875998 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-(4-bromobenzyl)-2,2-diethoxyacetimidamide (1.53 g, 4.85 mmol) in sulfuric acid (4 mL, 95-98%) was heated at 40 C for 14 h. The mixture was neutralized with 1 M NaOH to pH 7 and the resulting suspension was filtered. The residue was purified by silica gel chromatography with 20-55% ethyl acetate in hexanes. The desired fractions were concentrated to give a brownish yellow solid (0.434 g, 40%). LCMS: R.T.=1.62; [M+2]+=225.1.

WORKUP

后处理

  1. filtrationthe resulting suspension was filtered
  2. customThe residue was purified by silica gel chromatography with 20-55% ethyl acetate in hexanes
  3. concentrationThe desired fractions were concentrated