Pyridine → HCID 19860691, 화합물

HRID 868406노트

반응식

HRID 868406 반응식
[F:1][C:2]([F:8])([CH2:5][CH2:6][OH:7])[CH2:3][OH:4].N1C=CC=CC=1.[CH3:15][S:16](Cl)(=[O:18])=[O:17]>ClCCl>[CH3:15][S:16]([O:4][CH2:3][C:2]([F:8])([F:1])[CH2:5][CH2:6][O:7][S:16]([CH3:15])(=[O:18])=[O:17])(=[O:18])=[O:17]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 13935577108781-20-0

생성물 1

HCID 19860691HCID 19860691, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a stirred mixture of 2,2-difluoro-1,4-butanediol (12.97 g, 103 mM), dry pyridine (65 mL) and dichloromethane (200 mL), is slowly added a solution of methanesulfonyl chloride (23.6 g) in dichloromethane (50 mL). Stirring is continued overnight, and the mixture is washed with 2N HCl (twice), 10% aqueous NaHCO3 until neutral, and finally with water. The organic solution is dried (MgSO4) and evaporated to yield 1,4-bis-methanesulfonyloxy-2,2-difluorobutane as a slightly yellow oil (25.4 g, 87.5%) which crystallizes on scratching with dry ether: white crystals, 22.3 g (77%).

후처리

  1. washthe mixture is washed with 2N HCl (twice), 10% aqueous NaHCO3 until neutral, and finally with water
  2. dry with materialThe organic solution is dried (MgSO4)
  3. customevaporated

출처 및 근거

ORD 기록
ord-872d27ca3f2a4f1b95f227eda04b70e1
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04778926

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