Pyridine → HCID 19860691, 화합물

HRID 868409노트

반응식

HRID 868409 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 methanesulfonylchloride (23.6 g) in dichloromethane (50 mL). Stirring is continued overnight. The reaction mixture is washed with 2N HCl (twice), followed by 10% aqueous NaHCO3 until neutral, and then with water. The organic layer is dried (MgSO4) and upon evaporation of the solvents, a slightly yellow oil is obtained. Crystallization is induced by scratching the oil with dry ether, to yield the compound 1,4-bis-methanesulfonyloxy-2,2-difluorobutane as white crystals: 22.3 g (77%).

후처리

  1. washThe reaction mixture is washed with 2N HCl (twice),
  2. dry with materialThe organic layer is dried (MgSO4)
  3. customupon evaporation of the solvents
  4. customa slightly yellow oil is obtained
  5. customCrystallization

출처 및 근거

ORD 기록
ord-68accf6c674145728f9b0f11f3abd274
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04778926

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