HRID2203297

反应详情

EQUATION

反应方程式

HRID 2203297 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A flask was charged with (2-methyl-4-nitro-phenyl)-methanol (16.7 g, 0.100 mol) (334 mL), to manganese(IV) oxide (5 μm, 102.3 g, 1.00 mol), and CH2Cl2 (334 mL). The stirred mixture was heated at 40° C. for at least 2 h or until in-process HPLC analysis showed that conversion was greater than 95%. The cooled mixture was filtered through a celite cake (8 g) loaded onto a fritted funnel and the filter cake was rinsed with CH2Cl2 (340 mL). The filtrate and wash were concentrated under reduced pressure to dryness to afford the title compound as an amorphous solid (13.0 g, 78% yield).

WORKUP

后处理

  1. filtrationThe cooled mixture was filtered through a celite cake (8 g)
  2. customloaded onto a fritted funnel
  3. washthe filter cake was rinsed with CH2Cl2 (340 mL)
  4. washThe filtrate and wash
  5. concentrationwere concentrated under reduced pressure to dryness