Sodium borohydride → 5-[5-Bromo-4-(1-ethyl-2-hydroxy-propylsulfanyl)-pyrimidin-2-ylamino]-pyridine-2-sulfonic acid amide

HRID 1182062

反応式

HRID 1182062 の反応式
[Br:1][C:2]1[C:3]([S:19][CH:20]([CH2:24][CH3:25])[C:21](=[O:23])[CH3:22])=[N:4][C:5]([NH:8][C:9]2[CH:10]=[CH:11][C:12]([S:15]([NH2:18])(=[O:17])=[O:16])=[N:13][CH:14]=2)=[N:6][CH:7]=1.[BH4-].[Na+]>C1COCC1.CO.C(O)(=O)C>[Br:1][C:2]1[C:3]([S:19][CH:20]([CH2:24][CH3:25])[CH:21]([OH:23])[CH3:22])=[N:4][C:5]([NH:8][C:9]2[CH:10]=[CH:11][C:12]([S:15]([NH2:18])(=[O:17])=[O:16])=[N:13][CH:14]=2)=[N:6][CH:7]=1

参加物

5

反応物 2

HCID 4311764Sodium borohydrideHCID 589818355-[5-Bromo-4-(1-ethyl-2-oxo-propylsulfanyl)-pyrimidin-2-ylamino]-pyridine-2-sulfonic acid amide

生成物 1

HCID 589818875-[5-Bromo-4-(1-ethyl-2-hydroxy-propylsulfanyl)-pyrimidin-2-ylamino]-pyridine-2-sulfonic acid amide

試薬・触媒・溶媒 2

HCID 176Acetic Acid触媒HCID 21899815MeOH tetrahydrofuran溶媒

実験手順

26 mg (0.058 mmol) of 5-[5-bromo-4-(1-ethyl-2-oxo-propylsulfanyl)-pyrimidin-2-ylamino]-pyridine-2-sulfonic acid amide, dissolved in 1.5 ml of THF/MeOH 1:1, is mixed with 10 mg of sodium borohydride and stirred for 3 hours at room temperature. While being cooled, 2-3 drops of glacial acetic acid are added and concentrated by evaporation. Uptake in acetonitrile and suctioning-off yield 17 mg (65% of theory) of 5-[5-bromo-4-(1-ethyl-2-hydroxy-propylsulfanyl)-pyrimidin-2-ylamino]-pyridine-2-sulfonic acid amide.

後処理

  1. temperatureWhile being cooled
  2. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-8fe3323d05b246749d496264ffd29609
出典データセット
uspto-grants-2007_10
特許番号
US07288547B2

関連ノート

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