Methanesulfonyl chloride → 4-Pyrrolidinophenethyl mesylate

HRID 2251886

반응식

HRID 2251886 반응식
[N:1]1([C:6]2[CH:14]=[CH:13][C:9]([CH2:10][CH2:11][OH:12])=[CH:8][CH:7]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.[CH3:15][S:16](Cl)(=[O:18])=[O:17].C(=O)([O-])O.[Na+]>ClCCl>[S:16]([O:12][CH2:11][CH2:10][C:9]1[CH:13]=[CH:14][C:6]([N:1]2[CH2:5][CH2:4][CH2:3][CH2:2]2)=[CH:7][CH:8]=1)(=[O:18])(=[O:17])[CH3:15]

참가 물질

5

반응물 3

HCID 31297Methanesulfonyl chlorideHCID 516892Sodium BicarbonateHCID 12498372HCID 12498372, 화합물

생성물 1

HCID 229341624-Pyrrolidinophenethyl mesylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

4-Pyrrolidinophenethyl alcohol (16.41 g, 85.9 mmol) was dissolved in dichloromethane (150 ml). Dissopropylethylamine (19.0 ml, 108 ml) and methanesulfonyl chloride (8.40 ml, 108 mmol) were added to the obtained solution at 0° C., and they were stirred overnight. The reaction mixture was distributed into 5% aqueous sodium hydrogencarbonate solution and dichloromethane. The organic layer was dried and the solvent was evaporated under reduced pressure. The residue was subjected to the silica gel column chromatography. After the elution with hexane and ethyl acetate (7:3) as the eluent, suitable fractions were collected and the solvent was evaporated under reduced pressure to obtain 4-pyrrolidinophenethyl mesylate in the form of a white solid (21.14 g, 80%).

후처리

  1. customThe organic layer was dried
  2. customthe solvent was evaporated under reduced pressure
  3. washAfter the elution with hexane and ethyl acetate (7:3) as the eluent, suitable fractions
  4. customwere collected
  5. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-449dc1d5b6e8433f9450fc04471b8628
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07320973B2

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