HRID1981159
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
In 6 ml of acetone there was dissolved 90 mg of 2-amino-5,6-dichloro-3-(1-hydroxyethyl)pyrazine prepared in Step A above, after which there was added 360 mg of manganese dioxide, and the reaction mixture was stirred for 3 days at room temperature. The manganese dioxide was filtered off, and the precipitate washed three times with acetone, and then filtered. The filtrate was concentrated under vacuum and passed through a silica gel column, then eluted first with hexane, followed by 10% dichloromethane in hexane, with product in the first three fractions (53 mg).
WORKUP
后处理
- filtrationThe manganese dioxide was filtered off
- washthe precipitate washed three times with acetone
- filtrationfiltered
- concentrationThe filtrate was concentrated under vacuum
- washeluted first with hexane