HRID2257238

反应详情

EQUATION

反应方程式

HRID 2257238 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

25 mg of pTS acid are added to a solution of ethyl 3-phenyl-2-ethoxycarbonyl-2-(2-tetrahydropyranyloxy)-propanoate (6 g) in EtOH (25 ml). After 12 hours at r.t., the solvent is evaporated under vacuum, the mixture is partitioned between water and AcOEt; the organic phase is separated, dried, concentrated to small volume. The residue is adsorbed on SiO2 (40 g); by elution with 90:10 cyclohexane:AcOEt, 4.3 g of ethyl 3-phenyl-2-hydroxy-2-ethoxycarbonyl-propanoate, oil, are obtained. I.R.: 3500, 3000, 1740, 1600 cm-1 ; HNMR (CDCl3) δ (TMS): 1.2-1.35 t, 3.35 s, 3.15 s, 4.2-4.3 q, 7.25 s.

WORKUP

后处理

  1. customthe solvent is evaporated under vacuum
  2. customthe mixture is partitioned between water and AcOEt
  3. customthe organic phase is separated
  4. customdried
  5. concentrationconcentrated to small volume
  6. washby elution with 90:10 cyclohexane