Sodium Thiosulfate → HCID 484072、化合物

HRID 2287445ノート

反応式

HRID 2287445 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([OH:22])([CH2:16][N:17]1[CH:21]=[N:20][CH:19]=[N:18]1)[C:10](SCC)([F:12])[F:11].Cl[C:24]1C=CC=C(C(OO)=O)[CH:25]=1.[S:34]([O-:38])([O-])(=[O:36])=S.[Na+].[Na+].C(=O)(O)[O-].[Na+]>ClCCl.C(OCC)(=O)C>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([OH:22])([CH2:16][N:17]1[CH:21]=[N:20][CH:19]=[N:18]1)[C:10]([S:34]([CH2:24][CH3:25])(=[O:38])=[O:36])([F:12])[F:11]

参加物

7

反応物 4

HCID 24477Sodium ThiosulfateHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 10664501HCID 10664501、化合物

生成物 1

HCID 484072HCID 484072、化合物収率 78%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 2-(2,4-difluorophenyl)-1-(ethylthio)-1,1-difluoro-3-(1H-1,2,4-triazol-1-yl)-2-propanol (850 mg, 2.39 mmol) in dichloromethane (100 ml), 85% m-chloroperbenzoic acid (1.4 g, 5.75 mmol) was added at room temperature, followed by stirring at room temperature for 12 hours. After the completion of the reaction, a saturated aqueous solution of sodium thiosulfate and a saturated aqueous solution of sodium bicarbonate were added and the resulting mixture was stirred. The dichloromethane solution was separated and after washing with water, dried over magnesium sulfate. The solvent was then distilled off under reduced pressure. The residue so obtained was crystallized from isopropyl ether--ethyl acetate, whereby 2-(2,4-difluorophenyl)-1-(ethylsulfonyl)-1,1-difluoro-3-(1H-1,2,4-triazol-1-yl)-2-propanol (718 mg, yield: 78%) was obtained as colorless crystals.

後処理

  1. customAfter the completion of the reaction
  2. stirringthe resulting mixture was stirred
  3. customThe dichloromethane solution was separated
  4. washafter washing with water
  5. dry with materialdried over magnesium sulfate
  6. distillationThe solvent was then distilled off under reduced pressure
  7. customThe residue so obtained
  8. customwas crystallized from isopropyl ether

出典と根拠

ORDレコード
ord-b2ebb728b2544633a415d47b57303d8d
出典データセット
uspto-grants-2000_07
特許番号
US06083968

反応ノート

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