Water → HCID 178504858, 화합물

HRID 1500861노트

반응식

HRID 1500861 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 178504858HCID 178504858, 화합물수율 90%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-c09b0dfd6730461fa0fd6fd984cfbd7c
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09206191B2

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