HRID1013846
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 ethyl 2-(4-bromo-2-chlorobenzyl)-4-oxobutanoate (0.92 g, 2.8 mmol), 4,5,6,7-tetrahydro-1H-indazol-6-amine hydrochloride (preparation 80) (490 mg, 2.8 mmol) and sodium triacetoxyborohydride (886 mg, 4.2 mmol) in dichloroethane (50 mL) and stir for 48 hours at room temperature. Add water and extract with CH2Cl2. Dry the organic layer over magnesium sulfate, filter and concentrate. Purify the residue by silica gel chromatography affords the title compound (428 mg, 68%): MS (m/z): 410 (M+2).
WORKUP
后处理
- extractionAdd water and extract with CH2Cl2
- dry with materialDry the organic layer over magnesium sulfate
- filtrationfilter
- concentrationconcentrate
- customPurify the residue by silica gel chromatography