HRID2102994
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
CONDITIONS
反应条件
- 温度
- 200 °C
PROCEDURE
实验过程
A solution of 6-hydroxy-7,8-dimethyl-4H-spiro[chromene-3, 1′-cyclopropan]-4-one (10 mg), prepared as described above, methoxyamine hydrochloride (110 mg) in pyridine (3 mL) was stirred in a microwave reaction tube (200° C., 30 min). After cooling down, the mixture was partitioned between water and ethylacetate, and the organic layer was washed with dil. HCl, dried, and evaporated. The residue was purified by silica gel column eluting with 15% EtOAc in hexane to give a 3.6 mg of 6-hydroxy-7,8-dimethylspiro[chroman-3,1′-cyclopropan]-4-one O-methyl oxime.
WORKUP
后处理
- temperatureAfter cooling down
- customthe mixture was partitioned between water and ethylacetate
- washthe organic layer was washed with dil. HCl
- customdried
- customevaporated
- customThe residue was purified by silica gel column
- washeluting with 15% EtOAc in hexane