Triethylamine → 3-(4-Cyanophenyl)propyl methanesulfonate

HRID 485278ノート

反応式

HRID 485278 の反応式
[OH:1][CH2:2][CH2:3][CH2:4][C:5]1[CH:12]=[CH:11][C:8]([C:9]#[N:10])=[CH:7][CH:6]=1.C(N(CC)CC)C.[CH3:20][S:21](Cl)(=[O:23])=[O:22]>C(Cl)Cl>[S:21]([O:1][CH2:2][CH2:3][CH2:4][C:5]1[CH:6]=[CH:7][C:8]([C:9]#[N:10])=[CH:11][CH:12]=1)([CH3:20])(=[O:23])=[O:22]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 110841784-(3-Hydroxypropyl)benzonitrile

生成物 1

HCID 219936463-(4-Cyanophenyl)propyl methanesulfonate収率 100%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A 16.1 g (0.1 mol) quantity of 4-(3hydroxypropyl)benzonitrile was admixed with 27.8 ml (0.2 mol) of triethylamine and 300 ml of methylene chloride. To the mixture was added 15.5 ml (0.2 mol) of methanesulfonyl chloride at 0° C. The reaction mixture was stirred at room temperature for 12 hours and then concentrated. The concentrate was diluted with 500 ml of benzene, and washed with saturated aqueous solution of sodium chloride. The washed dilution was dried over Na2SO4 and concentrated, giving 24.0 g (yield 100%) of crude 4-(3-mesyloxypropyl)benzonitrile in the form of an oil.

後処理

  1. concentrationconcentrated
  2. additionThe concentrate was diluted with 500 ml of benzene
  3. washwashed with saturated aqueous solution of sodium chloride
  4. dry with materialThe washed dilution was dried over Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-c352a4f37f894099960436b4cd5e8b5f
出典データセット
uspto-grants-1985_08
特許番号
US04536391

反応ノート

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