HRID466766

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID24434

Potassium nitrate

KNO3

结构：C[C@H](CC[C@@H](C)C(C)(C)O)[C@H]1CC[C@H]2C3=CC=C4C[C@@H](O)C[C@H](O)[C@]4(C)[C@H]3CC[C@]12C

HCID23239490

未命名化合物

PRODUCTS

生成物

$结构：CC1=C(/C=C\C2=CCC[C@]3(C)[C@@H]([C@H](C)CCCC(C)C)CC[C@@H]23)C[C@@H](O)CC1$

HCID5281058

Previtamin D3

C27H44O

收率 28.3%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID3283

Diethyl Ether

C4H10O

PROCEDURE

实验过程

(24R)-5,7-Ergostadiene-1α,3β,25-triol (IIb) (100 mg, 0.23 mmol) prepared in Example 13 was dissolved in ether (1000 ml) and the solution was irradiated for 3 minutes with high pressure mercury lamp using 1.5% aqueous potassium nitrate solution as a filter under water-cooling in an argon gas stream. From the reaction solution was distilled off ether and the resultant residue was purified by preparative high performance liquid chromatography (HPLC) [column: LiChrosorb® Si60 (7 μm), φ25×250 mm, Merck Co., Ltd.; column effluent: 6% methanol-methylene chloride; flow rate: 6.0 ml/ml, detected at 265 nm] to give 25.0 mg of previtamin D (XIIb).

WORKUP

后处理

customthe solution was irradiated for 3 minutes with high pressure mercury lamp
filtrationa filter under water-
temperaturecooling in an argon gas stream
distillationFrom the reaction solution was distilled off ether
customthe resultant residue was purified by preparative high performance liquid chromatography (HPLC) [column