Water → 4-(methylthio)-1H-indazol-5-ol

HRID 1269926

반응식

HRID 1269926 반응식
FC(F)(F)C(O)=O.[CH3:8][S:9][C:10]1[C:18]([O:19]C2CCCCO2)=[CH:17][CH:16]=[C:15]2[C:11]=1[CH:12]=[N:13][N:14]2C1CCCCO1.O>ClCCl>[CH3:8][S:9][C:10]1[C:18]([OH:19])=[CH:17][CH:16]=[C:15]2[C:11]=1[CH:12]=[N:13][NH:14]2

참가 물질

5

반응물 3

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 694312114-(methylthio)-1-tetrahydro-2H-pyran-2-yl-5-(tetrahydro-2H-pyran-2-yloxy)-1H-indazole

생성물 1

HCID 229336484-(methylthio)-1H-indazol-5-ol수율 127.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Trifluoroacetic acid (1 ml) was added to a solution of 4-(methylthio)-1-tetrahydro-2H-pyran-2-yl-5-(tetrahydro-2H-pyran-2-yloxy)-1H-indazole (0.0730 g, 0.21 mmol) in dichloromethane (1 ml) and stirred for 1 hour. The reaction solution was added to water and extracted three times with ethyl acetate and the extract solution was dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue was purified by a silica gel chromatography (hexane/ethyl acetate=2/1), crystallized from hexane/ethyl acetate and then dried up to obtain 4-(methylthio)-1H-indazol-5-ol (0.0481 g, >99%).

후처리

  1. extractionextracted three times with ethyl acetate
  2. dry with materialthe extract solution was dried over anhydrous magnesium sulfate
  3. distillationThe solvent was distilled off
  4. customthe residue was purified by a silica gel chromatography (hexane/ethyl acetate=2/1)
  5. customcrystallized from hexane/ethyl acetate
  6. customdried up

출처 및 근거

ORD 기록
ord-859c810b4a29438a86d48865296117bc
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07199147B2

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