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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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Methanol → HCID 19036388、化合物

HRID 264546
ノート
印刷プレビュー

反応式

HRID 264546 の反応式
[CH2:1]([CH:5]1[CH2:14][CH2:13][C:12]2[C:7](=[C:8]([Cl:15])[CH:9]=[CH:10][CH:11]=2)[C:6]1=[O:16])[CH:2]=CC.C[OH:18]>ClCCl>[Cl:15][C:8]1[CH:9]=[CH:10][CH:11]=[C:12]2[C:7]=1[C:6](=[O:16])[CH:5]([CH2:1][CH:2]=[O:18])[CH2:14][CH2:13]2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 887MethanolHCID 543159702-(2-Buten-1-yl)-8-chloro-1-tetralone

生成物 1

HCID 19036388HCID 19036388、化合物収率 83%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

7.7 g of 2-(2-buten-1-yl)-8-chloro-1-tetralone were dissolved in a mixture of 220 ml of dichloromethane and 60 ml of methanol, cooled to -75° and the double bond was ozonized in the usual manner. After flushing the reaction mixture with oxygen and argon, 4.8 ml of dimethyl sulfide were added dropwise. The mixture was left to warm slowly to room temperature and was stirred for an additional 15 hours. The crude product (10.8 g) was dissolved in about 100 ml of dichloromethane and added to a mixture of 12 ml of 10% aqueous oxalic acid, 120 g of silica gel and 300 ml of dichloromethane. The mixture was stirred at room temperature for 2 hours. 6.4 g (83%) of 8-chloro-2-(2-oxoethyl)-1-tetralone were obtained as a pale brown oil by extraction with dichloromethane.

後処理

  1. temperaturecooled to -75°
  2. customAfter flushing the reaction mixture with oxygen and argon, 4.8 ml of dimethyl sulfide
  3. additionwere added dropwise
  4. waitThe mixture was left
  5. dissolutionThe crude product (10.8 g) was dissolved in about 100 ml of dichloromethane
  6. additionadded to a mixture of 12 ml of 10% aqueous oxalic acid, 120 g of silica gel and 300 ml of dichloromethane
  7. stirringThe mixture was stirred at room temperature for 2 hours

出典と根拠

ORDレコード
ord-4fb7c5fdc98843538413e4f5efd9223a
出典データセット
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05646173

反応ノート

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