Methanol → HCID 178509237, 화합물

HRID 1048810

반응식

HRID 1048810 반응식
[OH:1]OS([O-])=O.[K+].[F:7][C:8]1[CH:9]=[C:10]([S:15][C:16]2[CH:17]=[C:18]3[C:24]([NH2:25])=[N:23][NH:22][C:19]3=[N:20][CH:21]=2)[CH:11]=[C:12]([F:14])[CH:13]=1.O1CCCC1.CO.[OH2:33]>>[F:7][C:8]1[CH:9]=[C:10]([S:15]([C:16]2[CH:17]=[C:18]3[C:24]([NH2:25])=[N:23][NH:22][C:19]3=[N:20][CH:21]=2)(=[O:1])=[O:33])[CH:11]=[C:12]([F:14])[CH:13]=1

참가 물질

6

반응물 5

HCID 887MethanolHCID 962WaterHCID 8028TetrahydrofuranHCID 23707502Potassium hydroxy sulfite2회HCID 178509236HCID 178509236, 화합물

생성물 1

HCID 178509237HCID 178509237, 화합물수율 81%

실험 절차

A solution of 663 mg (1.078 mmol) of oxone in 1.1 ml of water is added to a solution of 300 mg (1.078 mmol) of 5-(3,5-difluorophenylthio)-1H-pyrazolo[3,4-b]pyridin-3-amine in 10 ml of a 1:1 mixture of tetrahydrofuran and methanol at 0° C. The reaction mixture is stirred at room temperature for 16 hours. An additional portion of 663 mg of oxone at 0° C. is then added and the reaction medium stirred at room temperature for 24 hours. The solvents are evaporated and the reaction medium is diluted with sodium bicarbonate solution, extracted with ethyl acetate, dried on MgSO4 and then concentrated to yield 340 mg (81%) of 5-(3,5-difluorophenylsulfonyl)-1H-pyrazolo[3,4-b]pyridin-3-amine in the form of a yellow solid.

후처리

  1. stirringthe reaction medium stirred at room temperature for 24 hours
  2. customThe solvents are evaporated
  3. additionthe reaction medium is diluted with sodium bicarbonate solution
  4. extractionextracted with ethyl acetate
  5. customdried on MgSO4
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e1bb9da3e2bc4b77912e8f432323058a
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09381195B2

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