Triethylamine → N-(2-Chloropropyl)-N,2,6-trimethylbenzenamine

HRID 1649976ノート

反応式

HRID 1649976 の反応式
CS([Cl:5])(=O)=O.[CH3:6][N:7]([CH2:16][CH:17](O)[CH3:18])[C:8]1[C:13]([CH3:14])=[CH:12][CH:11]=[CH:10][C:9]=1[CH3:15].C(N(CC)CC)C>ClCCCl>[CH3:6][N:7]([CH2:16][CH:17]([Cl:5])[CH3:18])[C:8]1[C:13]([CH3:14])=[CH:12][CH:11]=[CH:10][C:9]=1[CH3:15]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 13674770HCID 13674770、化合物

生成物 1

HCID 13674775N-(2-Chloropropyl)-N,2,6-trimethylbenzenamine収率 90.2%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

3.1 ml (4.6 g, 40 mmoles) of methanesulfonyl chloride are added dropwise, at a temperature not exceeding 20° C., to a solution of 7.0 g (36.2 mmoles) of 1-[N-methyl-N-(2,6-dimethylphenyl)-amino]-2-propanol and 5.45 ml (4.0 g, 40 mmoles) of triethyl amine in 50 ml of 1,2-dichloroethane, and the resulting mixture is stirred at room temperature for 3 hours. The mixture is washed then thrice with 30 ml of water, each, dried over anhydrous magnesium sulfate, the solvent is evaporated, and the oily residue is distilled under reduced pressure. 6.9 g (90.2%) of 1-[N-methyl-N-(2,6-dimethylphenyl)-amino]-2-chloro-propane are obtained; b.p.: 116°-118° C./133 Pa.

後処理

  1. washThe mixture is washed
  2. dry with materialeach, dried over anhydrous magnesium sulfate
  3. customthe solvent is evaporated
  4. distillationthe oily residue is distilled under reduced pressure

出典と根拠

ORDレコード
ord-92a3d90499da4f74afd93da2aa61e499
出典データセット
uspto-grants-1990_05
特許番号
US04922021

反応ノート

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