Triethylamine → 3-Methylsulfonylamino-1-methylsulfonyloxypropane

HRID 5471

반응식

HRID 5471 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][OH:5].C(N(CC)CC)C.[CH3:13][S:14](Cl)(=[O:16])=[O:15]>ClCCl>[CH3:13][S:14]([NH:1][CH2:2][CH2:3][CH2:4][O:5][S:14]([CH3:13])(=[O:16])=[O:15])(=[O:16])=[O:15]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 90863-Amino-1-propanolHCID 31297Methanesulfonyl chloride

생성물 1

HCID 233629523-Methylsulfonylamino-1-methylsulfonyloxypropane수율 69.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 3-amino-1-propanol (11.47 ml, 150 mmoles) and triethylamine (46 ml, 330 mmoles) in dichloromethane (250 ml) was added methylsulfonyl chloride (25.5 ml, 330 mmoles) with stirring under ice-cooling and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was washed in turn with an aqueous sodium bicarbnonate and water and dried. After the solvent was distilled off, the residue was purified by column chromatography (eluent: ethyl acetate) to obtain 24.22 g of the desired product (69.8%, white crystals).

후처리

  1. temperaturecooling
  2. stirringthe mixture was stirred at room temperature for 30 minutes
  3. washThe reaction mixture was washed in turn with an aqueous sodium bicarbnonate and water
  4. customdried
  5. distillationAfter the solvent was distilled off
  6. customthe residue was purified by column chromatography (eluent: ethyl acetate)

출처 및 근거

ORD 기록
ord-e88abdf757ee41b9b51549e401c0a380
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05244908

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