Methyl iodide → 4-[N-(4-Chloro-benzyl)-methylamino]-cyclohexanol

HRID 476959ノート

反応式

HRID 476959 の反応式
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][NH:7][CH:8]2[CH2:13][CH2:12][CH:11]([OH:14])[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[C:17](=O)([O-])[O-].[K+].[K+].CI>CN(C)C=O>[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][N:7]([CH3:17])[CH:8]2[CH2:9][CH2:10][CH:11]([OH:14])[CH2:12][CH2:13]2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 136706584-(4-Chloro-benzylamino)-cyclohexanol

生成物 1

HCID 136706604-[N-(4-Chloro-benzyl)-methylamino]-cyclohexanol

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

7.2 g (30 mMol) of 4-[N-(4-chloro-benzyl)-amino]-cyclohexanol are dissolved in 30 ml of dimethyl-formamide, and after the addition of 2.2 g (16 mMol) of potassium carbonate, 4.26 g (30 mMol) of methyliodide are added dropwise. When the slightly exothermic reaction has ended, the mixture is concentrated by evaporation, mixed with water and extracted with chloroform. The concentrated extracts are chromatographed on silica gel to purify them (eluant; methylene chloride/methanol=20/1).

後処理

  1. additionare added dropwise
  2. customWhen the slightly exothermic reaction
  3. concentrationthe mixture is concentrated by evaporation
  4. additionmixed with water
  5. extractionextracted with chloroform
  6. customThe concentrated extracts are chromatographed on silica gel
  7. customto purify them (eluant; methylene chloride/methanol=20/1)

出典と根拠

ORDレコード
ord-ea0f263269c04da98b88a92206933b76
出典データセット
uspto-grants-1989_12
特許番号
US04886812

反応ノート

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