HRID1013846

反应详情

EQUATION

反应方程式

HRID 1013846 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. extractionAdd water and extract with CH2Cl2
  2. dry with materialDry the organic layer over magnesium sulfate
  3. filtrationfilter
  4. concentrationconcentrate
  5. customPurify the residue by silica gel chromatography