Potassium Nitrate → Previtamin D3

HRID 466766

反応式

HRID 466766 の反応式
[CH3:1][C:2](O)([C@@H:4]([CH2:6][CH2:7][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>[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

参加物

4

反応物 2

HCID 24434Potassium NitrateHCID 23239490(24R)-5,7-Ergostadiene-1alpha,3beta,25-triol

生成物 1

HCID 5281058Previtamin D3収率 28.3%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

(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).

後処理

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

出典と根拠

ORDレコード
ord-33c56a26ac424946bb04bdff58915a7d
出典データセット
uspto-grants-1992_10
特許番号
US05157135

関連ノート

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