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
3-(4-(3-t-Butyldimethylsilyloxy-1-azetidinyl)-3-fluorophenyl)-5(R)-(isoxazol-3-yloxy methyl)oxazolidin-2-one (230 mg, 0.5 mmol) was dissolved in tetrahydrofuran (10 ml), and cooled under nitrogen to 0°. A solution of tetra-n-butylammonium fluoride (1 M, 1 ml, 1 mmol) was added and the mixture allowed to come to ambient temperature. Water (2 ml) was added, and the mixture evaporated to dryness. The residue was purified by chromatography on a 10 g silica Mega Bond Elut(D column, eluting with a gradient increasing in polarity from 0 to 2.5% MeOH in dichloromethane. Relevant fractions were combined and evaporated, then redissolved in EtOAc and the desired product (96 mg) precipitated by addition of isohexane.
WORKUP
后处理
- temperaturecooled under nitrogen to 0°
- customto come to ambient temperature
- customthe mixture evaporated to dryness
- customThe residue was purified by chromatography on a 10 g silica Mega Bond Elut(D column
- washeluting with a gradient
- temperatureincreasing in polarity from 0 to 2.5% MeOH in dichloromethane
- customevaporated
- dissolutionredissolved in EtOAc
- customthe desired product (96 mg) precipitated by addition of isohexane