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Isopropanol → octahydro-7a-methyl-1-[1-methyl-4-(2, 2,4-trimethyl-1,3-dioxolan-4-yl)-2-butenyl]-4H-inden-4-one

HRID 579814
ノート
印刷プレビュー

反応式

HRID 579814 の反応式
[CH3:1][C:2]12[CH:10]([CH:11]([CH3:23])[CH:12]=[CH:13][CH2:14][C:15]3([CH3:22])[CH2:19][O:18][C:17]([CH3:21])([CH3:20])[O:16]3)[CH2:9][CH2:8][CH:7]1[CH:6]([OH:24])[CH2:5][CH2:4][CH2:3]2.C([O-])(=O)C.[Na+].[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1C1C=CC=C[NH+]=1.[Cr](Cl)([O-])(=O)=O.C(O)(C)C>C(Cl)Cl.O>[CH3:1][C:2]12[CH:10]([CH:11]([CH3:23])[CH:12]=[CH:13][CH2:14][C:15]3([CH3:22])[CH2:19][O:18][C:17]([CH3:21])([CH3:20])[O:16]3)[CH2:9][CH2:8][CH:7]1[C:6](=[O:24])[CH2:5][CH2:4][CH2:3]2
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 3776IsopropanolHCID 517045Sodium AcetateHCID 76443847octahydro-7a-methyl-1-[1-methyl-4-(2,2,4-trimethyl-1,3-dioxolan-4-yl)-2-butenyl]-4H-inden-4-olHCID 178526115HCID 178526115、化合物2 回

生成物 1

HCID 76443494octahydro-7a-methyl-1-[1-methyl-4-(2, 2,4-trimethyl-1,3-dioxolan-4-yl)-2-butenyl]-4H-inden-4-one

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

A solution of 0.145 g of [1R-(1R*,2E,S*),1β,3aα,7aβ]-octahydro-7a-methyl-1-[1-methyl-4-(2,2,4-trimethyl-1,3-dioxolan-4-yl)-2-butenyl]-4H-inden-4-ol in 9 ml of dry methylene chloride was treated with 0.250 g of anhydrous sodium acetate and 0.500 g of 2,2'-bipyridinium chlorochromate and the mixture stirred at room temperature for two hours. After this time, an additional 0.250 g of 2,2'-bipyridinium chlorochromate was added and the stirring continued for two more hours. After this time, 0.5 ml of isopropyl alcohol was added and the mixture stirred for 15 minutes, then diluted with water, and extracted with 3×50 ml of ether. The combined organic phases were washed with water, dried and evaporated to dryness. The residue obtained was purified by chromatography on silica gel, eluting with hexane-ethyl acetate (3:1) to give 0.134 g (93%) of pure [1R-(1R*,2E,S*),1β,3 aα,7aβ]-octahydro-7a-methyl-1-[1-methyl-4-(2,2,4-trimethyl-1,3-dioxolan-4-yl)-2-butenyl]-4H-inden-4-one, [α]D25 (c 0.2, ethanol).

後処理

  1. stirringthe mixture stirred for 15 minutes
  2. extractionextracted with 3×50 ml of ether
  3. washThe combined organic phases were washed with water
  4. customdried
  5. customevaporated to dryness
  6. customThe residue obtained
  7. customwas purified by chromatography on silica gel
  8. washeluting with hexane-ethyl acetate (3:1)

出典と根拠

ORDレコード
ord-eae6f8f571674403bf061aa449fdf784
出典データセット
uspto-grants-1988_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04749710

反応ノート

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