HRID2108147

反应详情

EQUATION

反应方程式

HRID 2108147 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A two liter autoclave was charged with 130.6 g of N-(2,4-dinitrobenzoyl)morpholine, 1200 ml methanol and 6.2 g of a 5% palladium on carbon/50% water catalyst. The mixture was hydrogenated at 800 psi while maintaining the temperature between 60°-100° C. Hydrogen uptake ceased after 30 min. The mixture was cooled, filtered and methanol removed at reduced pressure. The residue was crystallized from toluene to yield 97.1 g of N-(2,4-diaminobenzoyl)morpholine, mp 114°-115° C.

WORKUP

后处理

  1. temperaturewhile maintaining the temperature between 60°-100° C
  2. temperatureThe mixture was cooled
  3. filtrationfiltered
  4. custommethanol removed at reduced pressure
  5. customThe residue was crystallized from toluene