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

Benzyl Alcohol → 3-(5-Benzyloxypentyl)-7,7-ethylenedioxy-3-hydroxy-cis-bicyclo[3,3,0]octane

HRID 1654244
ノート
印刷プレビュー

反応式

HRID 1654244 の反応式
[CH2:1]1[CH2:13][O:12][C:3]2([CH2:10][C@@H:9]3[C@@H:5]([CH2:6][C:7](=[O:11])[CH2:8]3)[CH2:4]2)[O:2]1.[CH2:14]([O:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26]Br)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[Mg].C(Br)CCCCBr.C(O)C1C=CC=CC=1.[Cl-].[NH4+]>C(OCC)C>[CH2:14]([O:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][C:7]1([OH:11])[CH2:6][C@@H:5]2[C@@H:9]([CH2:10][C:3]3([O:2][CH2:1][CH2:13][O:12]3)[CH2:4]2)[CH2:8]1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 6

HCID 244Benzyl AlcoholHCID 81001,5-DibromopentaneHCID 25517Ammonium ChlorideHCID 5462224MagnesiumHCID 11030443(3'aR,6'aS)-hexahydro-1'H-spiro(1,3-dioxolane-2,2'-pentalen)-5'-oneHCID 14221121Benzyl 5-Bromoamyl Ether2 回

生成物 1

HCID 22852672
3-(5-Benzyloxypentyl)-7,7-ethylenedioxy-3-hydroxy-cis-bicyclo[3,3,0]octane
収率 56.1%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A solution of 501 mg of 7,7-ethylenedioxy-3-oxo-cis-bicyclo[3,3,0]octane in 5 ml of diethyl ether was added dropwise at room temperature to 5-benzyloxypentamethylene-magnesium bromide, which had been prepared in 5 ml of diethyl ether from 1.00 g of 5-benzyloxypentyl bromide and 100 mg of metallic magnesium at room temperature. The 5-benzyloxypentyl bromide, in turn, had been prepared from pentamethylene bromide and benzyl alcohol according to the method of A. W. Burgstabler et al. [J. Org. Chem. 42, 566 (1977)]. The mixture was stirred for 1.5 hours at room temperature. Upon completion of the reaction, an aqueous solution of ammonium chloride was added to the reaction mixture, which was then extracted with diethyl ether. The extract was washed with water and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, giving 1.47 of residue. On purifying the residues by silica gel column chromatography, 556 mg of the title compound were obtained as an oil from the fractions eluted with hexane containing 25-30% by volume of ethyl acetate.

後処理

  1. customUpon completion of the reaction
  2. extractionwas then extracted with diethyl ether
  3. washThe extract was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. customgiving 1.47 of residue
  7. customOn purifying the residues by silica gel column chromatography

出典と根拠

ORDレコード
ord-7a981fc9f16a43009223f252d055b749
出典データセット
uspto-grants-1995_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05405870

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