Lithium hydroxide, monohydrate → HCID 10665616、化合物

HRID 1585666ノート

反応式

HRID 1585666 の反応式
C([O:4][CH2:5][CH2:6][S:7][C:8]([F:26])([F:25])[C:9]([C:17]1[CH:22]=[CH:21][C:20]([F:23])=[CH:19][C:18]=1[F:24])([OH:16])[CH2:10][N:11]1[CH:15]=[N:14][CH:13]=[N:12]1)(=O)C.O.[OH-].[Li+]>C(O)C>[F:24][C:18]1[CH:19]=[C:20]([F:23])[CH:21]=[CH:22][C:17]=1[C:9]([OH:16])([CH2:10][N:11]1[CH:15]=[N:14][CH:13]=[N:12]1)[C:8]([F:26])([F:25])[S:7][CH2:6][CH2:5][OH:4]

参加物

4

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 108343901-(2-acetoxyethyl)thio-2-(2,4-difluorophenyl)-1,1-difluoro-3-(1H-1,2,4-triazol-1-yl)propan-2-ol

生成物 1

HCID 10665616HCID 10665616、化合物収率 89.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 1-(2-acetoxyethyl)thio-2-(2,4-difluorophenyl)-1,1-difluoro-3-(1H-1,2,4-triazol-1-yl)propan-2-ol (14.3 g, 0.12 mol) in ethanol (200 ml), a 10% aqueous solution (20 ml) of lithium hydroxide monohydrate was added and they were stirred at room temperature for one hour. After the completion of the reaction, the reaction mixture was distilled off under reduced pressure. Water was added to the residue so obtained, followed by extraction with chloroform. The chloroform solution was washed with water, dried over magnesium sulfate and then distilled off under reduced pressure, whereby 2-(2,4-difluorphenyl)-1,1-difluoro-1-(2-hydroxyethyl)thio-3-(1H-1,2,4-triazol-1-yl)propan-2-ol (11.4 g, yield: 89.8%) was obtained as colorless crystals.

後処理

  1. customAfter the completion of the reaction
  2. distillationthe reaction mixture was distilled off under reduced pressure
  3. additionWater was added to the residue
  4. customso obtained
  5. extractionfollowed by extraction with chloroform
  6. washThe chloroform solution was washed with water
  7. dry with materialdried over magnesium sulfate
  8. distillationdistilled off under reduced pressure

出典と根拠

ORDレコード
ord-7d17324f792e4d05a1625b73aec87109
出典データセット
uspto-grants-1999_08
特許番号
US05939448

反応ノート

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