HRID330550
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
- 50 °C
PROCEDURE
实验过程
Potassium nitrosodisulfonate (12 g) and sodium acetate (12 g) are suspended in methanol-water (5:2, 210 ml), and 11-(2-hydroxy-3,4-dimethoxy-6-methylpheyl)-2-methylundecan-2-ol (2.4 g) is added thereto. The mixture is stirred at 50° C. for 14 hours and then diluted with water (100 ml). The methanol is distilled off. The aqueous soliution is extracted with ethyl acetate (200 ml), and the extract is washed with water, dried and concentrated under reduced pressure. The residue is subjected to silica gel column chromatography to give 1.7 g of 6-(10-hydroxy-10-methylundecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone as an orange oil.
WORKUP
后处理
- distillationThe methanol is distilled off
- extractionThe aqueous soliution is extracted with ethyl acetate (200 ml)
- washthe extract is washed with water
- customdried
- concentrationconcentrated under reduced pressure