HRID1534198

反应详情

EQUATION

反应方程式

HRID 1534198 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(24R,22E)-5,7,22-Ergostatrien-1α,3β,25-triol (Ib) (100 mg, 0.23 mmol) was dissolved in a mixed solution of ether (950 ml) and tetrahydrofuran (50 ml), and the solution was irradiated with high pressure mercury lamp using an 1.5% aqueous potassium nitrate solution as a filter with water cooling in a nitrogen stream for 3 minutes. The residue obtained by distilling off the solvent from the reaction solution was purified by HPLC (column: Lichrosorb® Si60 (7 μm), φ25×250 mm, Merck Co., Ltd.; column effluent: 5% methanol/methylene chloride; flow rate: 8.0 ml/min; detected at 265 nm) to give 28 mg of the previtamin D.

WORKUP

后处理

  1. customthe solution was irradiated with high pressure mercury lamp
  2. filtrationa filter with water cooling in a nitrogen stream for 3 minutes
  3. customThe residue obtained
  4. distillationby distilling off the solvent from the reaction solution
  5. customwas purified by HPLC (column