HRID1167430

反应详情

EQUATION

反应方程式

HRID 1167430 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturecooled under nitrogen to 0°
  2. customto come to ambient temperature
  3. customthe mixture evaporated to dryness
  4. customThe residue was purified by chromatography on a 10 g silica Mega Bond Elut(D column
  5. washeluting with a gradient
  6. temperatureincreasing in polarity from 0 to 2.5% MeOH in dichloromethane
  7. customevaporated
  8. dissolutionredissolved in EtOAc
  9. customthe desired product (96 mg) precipitated by addition of isohexane