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Water → 1-(2-Chloromethylcyclohex-1-enyl)-3-nitrobenzene

HRID 1693152
ノート
印刷プレビュー

反応式

HRID 1693152 の反応式
C(N(CC)C(C)C)(C)C.[N+:10]([C:13]1[CH:14]=[C:15]([C:19]2[CH2:24][CH2:23][CH2:22][CH2:21][C:20]=2[CH2:25]O)[CH:16]=[CH:17][CH:18]=1)([O-:12])=[O:11].CS([Cl:31])(=O)=O.O>ClCCl>[Cl:31][CH2:25][C:20]1[CH2:21][CH2:22][CH2:23][CH2:24][C:19]=1[C:15]1[CH:16]=[CH:17][CH:18]=[C:13]([N+:10]([O-:12])=[O:11])[CH:14]=1
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 962WaterHCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 57827168[2-(3-Nitrophenyl)cyclohex-1-enyl]methanol

生成物 1

HCID 578277541-(2-Chloromethylcyclohex-1-enyl)-3-nitrobenzene

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

N,N-Diisopropylethylamine (3.64 mL) was added to a solution of [2-(3-nitrophenyl)cyclohex-1-enyl]methanol obtained in Preparation Example 4-(2) (1.67 g) in dichloromethane (109 mL) in an ice bath. Then, methanesulfonyl chloride (668 μL) was added dropwise. The reaction mixture was warmed to room temperature and stirred overnight. Water was added to the reaction mixture, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate. The drying agent was removed by filtration and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography to obtain the title compound (1.56 g).

後処理

  1. extractionfollowed by extraction with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. customThe drying agent was removed by filtration
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-982cf035f9a847e186536dcdfaac3a74
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08158620B2

反応ノート

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