HRID132227
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
(S)-dimethyl 2-((7-bromo-4-(hydroxymethyl)-1H-indazol-5-yl)methyl)succinate (2.25 g, 5.8 mmol) was dissolved in 2M thionyl chloride in dichloromethane (42 mL, 84 mmol). Reaction stirred at room temperature for 2.0 hours. Mixture was concentrated. Residue was treated with toluene and then concentrated by roto-vap. Residue was dissolved in ethyl acetate. Mixture was washed twice with aqueous sodium bicarbonate. Organic was dried (magnesium sulfate), filtered and concentrated in vacuo. Title compound was obtained as amber solid in 99% yield.
WORKUP
后处理
- customReaction
- concentrationMixture was concentrated
- additionResidue was treated with toluene
- concentrationconcentrated by roto-vap
- dissolutionResidue was dissolved in ethyl acetate
- washMixture was washed twice with aqueous sodium bicarbonate
- dry with materialOrganic was dried (magnesium sulfate)
- filtrationfiltered
- concentrationconcentrated in vacuo