HRID17840

反应详情

EQUATION

反应方程式

HRID 17840 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 4-cyclopropyl-7-nitro-4H-1,2,4-benzothiadiazine 1,1-dioxide (5 g; prepared in Step C of Example 41) in ethanol (180 mL) there is added 10 % palladium-on-carbon (500 mg). The suspension is placed in a hydrogenator under 10 atmospheres of H2 for 30 minutes at ambient temperature. The suspension is concentrated to dryness under reduced pressure and the residue is taken up in boiling acetone (300 mL). The insoluble material is removed by filtration in the hot state and is washed with boiling acetone. The filtrate is concentrated to dryness and the residue is recrystallised from methanol.

WORKUP

后处理

  1. concentrationThe suspension is concentrated to dryness under reduced pressure
  2. customThe insoluble material is removed by filtration in the hot state
  3. washis washed with boiling acetone
  4. concentrationThe filtrate is concentrated to dryness
  5. customthe residue is recrystallised from methanol