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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
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Ethylene Glycol → 1,4-Dioxaspiro[4.5]decane, 8-[4-(3,4-difluorophenyl)-3-cyclohexen-1-yl]-

HRID 2081521
ノート
印刷プレビュー

反応式

HRID 2081521 の反応式
[F:1][C:2]1[CH:3]=[C:4]([C:9]2(O)[CH2:14][CH2:13][CH:12]([CH:15]3[CH2:24][CH2:23][C:18]4([O:22][CH2:21][CH2:20][O:19]4)[CH2:17][CH2:16]3)[CH2:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[F:8].C(O)CO.C[Si](O[Si](C)(C)C)(C)C.[O-2].[Al+3].[O-2].[O-2].[Al+3]>C(Cl)CCl>[F:1][C:2]1[CH:3]=[C:4]([C:9]2[CH2:14][CH2:13][CH:12]([CH:15]3[CH2:24][CH2:23][C:18]4([O:19][CH2:20][CH2:21][O:22]4)[CH2:17][CH2:16]3)[CH2:11][CH:10]=2)[CH:5]=[CH:6][C:7]=1[F:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 174Ethylene GlycolHCID 24764HexamethyldisiloxaneHCID 9989226AluminaHCID 190011474-[4-Hydroxy-4-(3,4-difluorophenyl)cyclohexyl]cyclohexanone ethyleneacetal

生成物 1

HCID 115590611,4-Dioxaspiro[4.5]decane, 8-[4-(3,4-difluorophenyl)-3-cyclohexen-1-yl]-収率 66.2%

試薬・触媒・溶媒 1

HCID 11
1,2-Dichloroethane
溶媒

実験手順

A mixture of 7.8 g of crude 1-(3,4-difluorophenyl)-4-(1,4-dioxa-8-spiro[4.5]decyl) cyclohexanol, 1.05 ml of ethylene glycol, 1.05 g of Amberlyst® 15 (strongly acid ion exchange resin, Fluka AG) and 80 ml of ethylene chloride was refluxed through neutral aluminum oxide for 3 hours. Subsequently, the mixture was cooled to room temperature and washed twice with water. The aqueous phases were extracted twice with methylene chloride. The organic phases where dried over sodium sulfate, filtered and concentrated. Chromatographic purification of the residue on silica gel with hexane/ethyl acetate (vol. 96:4) gave 4,9 g of 8-[4-(3,4-difluorophenyl)-3-cyclohexenyl]-1,4-dioxaspiro [4.5]decane as colorless crystals.

後処理

  1. washwashed twice with water
  2. extractionThe aqueous phases were extracted twice with methylene chloride
  3. dry with materialThe organic phases where dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customChromatographic purification of the residue on silica gel with hexane/ethyl acetate (vol. 96:4)

出典と根拠

ORDレコード
ord-5f710469012a4e4f8fa2477df165a849
出典データセット
uspto-grants-1993_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05185098

反応ノート

読み込み中…

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