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

HRID 1269926

反応式

HRID 1269926 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-859c810b4a29438a86d48865296117bc
出典データセット
uspto-grants-2007_04
特許番号
US07199147B2

関連ノート

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