HRID10091

反应详情

EQUATION

反应方程式

HRID 10091 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-Butylamino-5-nitro-10-aza-tricyclo[6.3.1.02,7]dodeca-2(7),3,5-triene-10-carboxlic acid tert-butyl ester (460 mg, 1.27 mmol) was treated with ammonium formate (850 mg, 12.7 mmol) and 10%Pd(OH)2/C (50 mg) in methanol (20 mL) and brought to reflux for 1 hour then filtered through a Celite pad and concentrated. The solids were treated with saturated aqueous Na2CO3 solution, extracted with CH2Cl2 (3×30 mL) and dried by filtration through a cotton plug to give an oil (440 mg, 100%).

WORKUP

后处理

  1. temperatureto reflux for 1 hour
  2. filtrationthen filtered through a Celite pad
  3. concentrationconcentrated
  4. additionThe solids were treated with saturated aqueous Na2CO3 solution
  5. extractionextracted with CH2Cl2 (3×30 mL)
  6. customdried by filtration through a cotton plug