Pyridine → HCID 19860691、化合物

HRID 868409ノート

反応式

HRID 868409 の反応式
[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]

参加物

5

反応物 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 13935577108781-20-0

生成物 1

HCID 19860691HCID 19860691、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-68accf6c674145728f9b0f11f3abd274
出典データセット
uspto-grants-1988_10
特許番号
US04778926

反応ノート

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