Potassium Nitrate → Previtamin D3

HRID 1534198노트

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HRID 1534198 반응식
[CH3:1][C:2](O)([C@@H:4](/[CH:6]=[CH:7]/[C@H:8]([C@@H:10]1[C@:27]2([CH3:28])[C@H:13]([C:14]3[C@H:24]([CH2:25][CH2:26]2)[C@:22]2([CH3:23])[C:17]([CH2:18][C@@H:19]([OH:30])[CH2:20][C@@H:21]2O)=[CH:16][CH:15]=3)[CH2:12][CH2:11]1)[CH3:9])C)[CH3:3].[N+]([O-])([O-])=O.[K+]>CCOCC.O1CCCC1>[CH3:23][C:22]1[CH2:21][CH2:20][C@H:19]([OH:30])[CH2:18][C:17]=1/[CH:16]=[CH:15]\[C:14]1[C@@H:13]2[CH2:12][CH2:11][C@H:10]([C@@H:8]([CH2:7][CH2:6][CH2:4][CH:2]([CH3:3])[CH3:1])[CH3:9])[C@@:27]2([CH3:28])[CH2:26][CH2:25][CH:24]=1

참가 물질

5

반응물 2

HCID 24434Potassium NitrateHCID 678319321,25-Dihydroxylumisterol(3)

생성물 1

HCID 5281058Previtamin D3수율 31.7%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

실험 절차

(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.

후처리

  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

출처 및 근거

ORD 기록
ord-86760e10313e4582b8e26cf079ad942b
출처 데이터셋
uspto-grants-1992_02
특허 번호
US05087709

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