Lithium hydroxide, monohydrate → HCID 10665616, 화합물

HRID 1585666노트

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HRID 1585666 반응식
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]

참가 물질

4

반응물 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

생성물 1

HCID 10665616HCID 10665616, 화합물수율 89.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7d17324f792e4d05a1625b73aec87109
출처 데이터셋
uspto-grants-1999_08
특허 번호
US05939448

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