Water → HCID 178504858、化合物

HRID 1500861ノート

反応式

HRID 1500861 の反応式
[CH3:1][S:2][C:3]1[C:11]2[C:6](=[CH:7][N:8]=[CH:9][CH:10]=2)[NH:5][N:4]=1.[OH:12]OS([O-])=O.[K+].[OH2:18]>CN(C=O)C>[CH3:1][S:2]([C:3]1[C:11]2[C:6](=[CH:7][N:8]=[CH:9][CH:10]=2)[NH:5][N:4]=1)(=[O:12])=[O:18]

参加物

5

反応物 3

HCID 962WaterHCID 23707502Potassium hydroxy sulfiteHCID 899242963-(methylthio)-1H-pyrazolo[3,4-c]pyridine

生成物 1

HCID 178504858HCID 178504858、化合物収率 90%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 3-(methylthio)-1H-pyrazolo[3,4-c]pyridine (10 g, 60.6 mmol) in DMF (100 mL) was added oxone (37 g, 121.2 mmol.) in portions. The reaction mixture was stirred at RT. After the reaction completed, water (100 mL) was added. The reaction was quenched carefully by addition of Na2SO3 and Na2CO3. The solid was filtered off and washed with MeOH (300 mL). The filtrate was concentrated under vacuum and the residue was purified by chromatography on silica gel column (DCM/MeOH=20/1) to give 3-(methylsulfonyl)-1H-pyrazolo[3,4-c]pyridine (10.7 g, yield: 90%) as a yellow solid. MS obsd. (ESI+) [(M+H)+] 198.0.

後処理

  1. customThe reaction was quenched carefully by addition of Na2SO3 and Na2CO3
  2. filtrationThe solid was filtered off
  3. washwashed with MeOH (300 mL)
  4. concentrationThe filtrate was concentrated under vacuum
  5. customthe residue was purified by chromatography on silica gel column (DCM/MeOH=20/1)

出典と根拠

ORDレコード
ord-c09b0dfd6730461fa0fd6fd984cfbd7c
出典データセット
uspto-grants-2015_12
特許番号
US09206191B2

反応ノート

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