Triethylamine → 3-(4-Cyanophenyl)propyl methanesulfonate

HRID 485278노트

반응식

HRID 485278 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 219936463-(4-Cyanophenyl)propyl methanesulfonate수율 100%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c352a4f37f894099960436b4cd5e8b5f
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04536391

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