HRID1013821
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureCool
- customthe reaction
- filtrationfilter through hyflo
- customRemove the solvent in vacuo
- custompurify the crude product with 10% 2 M NH3 in MeOH in CH2Cl2
- customre-purify
- additionmixed fractions with 15% 2 M NH3 in MeOH in CH2Cl2