ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

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

HRID 892784
ノート
印刷プレビュー

反応式

HRID 892784 の反応式
[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1C1C=CC=C[NH+]=1.[Cr](Cl)([O-])(=O)=O.C([O-])(=O)C.[Na+].[CH3:28][C:29]12[CH:37]([CH:38]([CH3:50])[CH2:39][CH2:40][CH2:41][C:42]3([CH3:49])[CH2:46][O:45][C:44]([CH3:48])([CH3:47])[O:43]3)[CH2:36][CH2:35][CH:34]1[CH:33]([OH:51])[CH2:32][CH2:31][CH2:30]2.CC(O)C>C(Cl)Cl.O>[CH3:28][C:29]12[CH:37]([CH:38]([CH3:50])[CH2:39][CH2:40][CH2:41][C:42]3([CH3:49])[CH2:46][O:45][C:44]([CH3:48])([CH3:47])[O:43]3)[CH2:36][CH2:35][CH:34]1[C:33](=[O:51])[CH2:32][CH2:31][CH2:30]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 14180908octahydro-7a-methyl-1-[1-methyl-4-(2,2,4-trimethyl-1,3-dioxolan-4-yl) butyl]-1H-inden-4-olHCID 178526115HCID 178526115、化合物2 回

生成物 1

HCID 14180910octahydro-7a-methyl-1-[1-methyl-4-(2,2, 4-trimethyl-1,3-dioxolan-4-yl)-butyl]-4H-inden-4-one収率 90%

試薬・触媒・溶媒

2
HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

To a suspension of 1.720 g of 2,2'-bipyridinium chlorochromate and 0.860 g of anhydrous sodium acetate in 10 ml of methylene chloride, was added a solution of 0.500 g of [1R-[1β(R*,S*),3aα,4β,7aβ]]-octahydro-7a-methyl-1-[1-methyl-4-(2,2,4-trimethyl-1,3-dioxolan-4-yl) butyl]-1H-inden-4-ol in 5 ml of methylene chloride and the mixture obtained stirred at room temperature for 2 hours. Additional 0.800 g of 2,2'-bipyridinium chlorochromate was then added and the stirring continued for an additional 2.5 hours. After this time, 1 ml of 2-propanol was introduced and 15 minutes later, the mixture diluted with water and extracted with ether. The combined organic phases were dried, evaporated and the residue purified by fast filtration through silica (eluent: hexane-ethyl acetate, 3:1) to give 0.446 g (90% yield) of pure [1R-(1R*,S*)-1β,3aα,7aβ ]-octahydro-7a-methyl-1-[1-methyl-4-(2,2,4-trimethyl-1,3-dioxolan-4-yl)-butyl]-4H-inden-4-one.

後処理

  1. customthe mixture obtained
  2. waitthe stirring continued for an additional 2.5 hours
  3. extractionextracted with ether
  4. customThe combined organic phases were dried
  5. customevaporated
  6. filtrationthe residue purified by fast filtration through silica (eluent: hexane-ethyl acetate, 3:1)

出典と根拠

ORDレコード
ord-1ec3f2d2a2c74d4697fd5bf75eefe42d
出典データセット
uspto-grants-1992_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05120722

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート