HRID1037547
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
A mixture of Compound (6) (92 mg, 0.14 mmol) and hydrazine hydrate (0.15 mL) in ethanol (7 mL) was stirred at RT for 16 h. The resulting suspension was filtered and the filtrate was concentrated to give a crude oil which then was partitioned between EtOAc (5 mL) and water (2 mL). The organic phase was separated and the aqueous phase was extracted with EtOAc (3×3 mL). The combined organic phase was dried (MgSO4) and the solvent was removed in vacuo to give 6-[(2-aminoethyl)(methylsulfonyl)amino]-2-(4-bromophenyl)-5-cyclopropyl-N-methyl-2H-indazole-3-carboxamide (7) (68 mg, 93%). ESI-MS m/z calculated for [M+H]+: 506.08/508.09; found: 505.88/507.89.
WORKUP
后处理
- filtrationThe resulting suspension was filtered
- concentrationthe filtrate was concentrated
- customto give a crude oil which
- customthen was partitioned between EtOAc (5 mL) and water (2 mL)
- customThe organic phase was separated
- extractionthe aqueous phase was extracted with EtOAc (3×3 mL)
- dry with materialThe combined organic phase was dried (MgSO4)
- customthe solvent was removed in vacuo