Methanol → HCID 178509237、化合物

HRID 1048810

反応式

HRID 1048810 の反応式
[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

参加物

6

反応物 5

HCID 887MethanolHCID 962WaterHCID 8028TetrahydrofuranHCID 23707502Potassium hydroxy sulfite2 回HCID 178509236HCID 178509236、化合物

生成物 1

HCID 178509237HCID 178509237、化合物収率 81%

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e1bb9da3e2bc4b77912e8f432323058a
出典データセット
uspto-grants-2016_07
特許番号
US09381195B2

関連ノート

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