HRID7872
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
A solution of (2SR,9aSR)-2-allyl-9a-butyl-7-methoxymethoxy-4-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one (5 mg, 0.015 mmol) in THF (0.5 mL) was treated with 6N HCl (0.5 mL) and the resulting solution was heated at 50° C. overnight. The mixture was diluted with EtOAc (30 mL), washed with 5% NaHCO3 and brine, dried over MgSO4, filtered, and evaporated under vacuum to a yellow oil. The crude product was purified by PLC on a 0.025×20×20 cm silica gel GF plate using 2:1 hexanes-EtOAc as developing solvent. The UV visible band at Rf 0.43-0.57 afforded (2SR,9aSR)-2-allyl-9a-butyl-7-hydroxy-4-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one as a gum.
WORKUP
后处理
- washwashed with 5% NaHCO3 and brine
- dry with materialdried over MgSO4
- filtrationfiltered
- customevaporated under vacuum to a yellow oil
- customThe crude product was purified by PLC on a 0.025×20×20 cm silica gel GF plate