HRID1055282
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In a 1000 mL round flask, 9,9-dihexyl-2-methyl-2,3-dihydrocyclopenta[b]fluoren-1(9H)-one (85 g, 211.1 mmol) was dissolved in 400 mL of THF and 400 mL of ethanol and then stirred. Sodium borohydride (NaBH4) (10 g, 265.0 mmol) was added to the reactant in five lots, and then stirred for 12 hours. After removal of the solvent, the resultant material was dissolved in ethylacetate, and then washed with water three times. The organic layer was dried over magnesium sulfate, followed by removal of volatile materials and drying, thereby obtaining 82.0 g of 9,9-dihexyl-2-methyl-1,2,3,9-tetrahydrocyclopenta[b]fluoren-1-ol (yield: 96.0%) (two isomers) as highly viscous oil.
WORKUP
后处理
- customAfter removal of the solvent
- dissolutionthe resultant material was dissolved in ethylacetate
- washwashed with water three times
- dry with materialThe organic layer was dried over magnesium sulfate
- customfollowed by removal of volatile materials
- customdrying