HRID1013821

反应详情

EQUATION

反应方程式

HRID 1013821 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Combine 1H-indazol-6-ylamine (12.45 g, 93.6 mmol) and 5% Rh/C (6.13 g) in ethanol (300 mL) and heat at 120° C. for 72 hours under ˜1000 psi H2. Cool the reaction and filter through hyflo. Remove the solvent in vacuo and purify the crude product with 10% 2 M NH3 in MeOH in CH2Cl2 and re-purify mixed fractions with 15% 2 M NH3 in MeOH in CH2Cl2 to afford 4.80 g (37%) of the titled product. MS (m/z): 138 (M+1).

WORKUP

后处理

  1. temperatureCool
  2. customthe reaction
  3. filtrationfilter through hyflo
  4. customRemove the solvent in vacuo
  5. custompurify the crude product with 10% 2 M NH3 in MeOH in CH2Cl2
  6. customre-purify
  7. additionmixed fractions with 15% 2 M NH3 in MeOH in CH2Cl2