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Sodium hydride → HCID 57964957、化合物

HRID 1931775
ノート
印刷プレビュー

反応式

HRID 1931775 の反応式
[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][CH:6]=1)(=[O:4])=[O:3].[H-].[Na+].[C:14]([O:18][C:19]([N:21]1[CH2:26][CH2:25][CH:24]([N:27]2[C:31]3=[N:32][C:33]([Cl:37])=[N:34][C:35](Cl)=[C:30]3[CH:29]=[N:28]2)[CH2:23][CH2:22]1)=[O:20])([CH3:17])([CH3:16])[CH3:15].[Cl-].[NH4+]>O1CCCC1>[C:14]([O:18][C:19]([N:21]1[CH2:26][CH2:25][CH:24]([N:27]2[C:31]3=[N:32][C:33]([Cl:37])=[N:34][C:35]([O:11][C:8]4[CH:9]=[CH:10][C:5]([S:2]([CH3:1])(=[O:3])=[O:4])=[CH:6][CH:7]=4)=[C:30]3[CH:29]=[N:28]2)[CH2:23][CH2:22]1)=[O:20])([CH3:17])([CH3:15])[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 1233504-(Methylsulfonyl)phenolHCID 57964878HCID 57964878、化合物2 回

生成物 1

HCID 57964957HCID 57964957、化合物収率 66.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒

実験手順

A solution of 4-(methylsulfonyl)phenol (available from Matrix Scientific, Columbia, S.C., USA; 52 mg, 0.3 mmol) in tetrahydrofuran (3 mL) was cooled to 0° C. under argon. Sodium hydride (60% dispersion; 13.2 mg, 0.33 mmol) was added and the mixture was stirred for 10 min. 4-(4,6-Dichloro-pyrazolo[3,4-d]pyrimidin-1-yl)-piperidine-1-carboxylic acid tert-butyl ester (Intermediate 24; 100 mg, 0.27 mmol) was added and the mixture was stirred at room temperature for 4 h and then poured into saturated aqueous ammonium chloride solution. The mixture was extracted three times with ethyl acetate and the combined organic layers were washed with brine, dried (magnesium sulfate), filtered, evaporated and purified by column chromatography, eluting with 25-50% ethyl acetate/hexanes to give 4-[6-chloro-4-(4-methanesulfonyl-phenoxy)-pyrazolo[3,4-d]pyrimidin-1-yl]-piperidine-1-carboxylic acid tert-butyl ester (91 mg, 66%) as a white solid.

後処理

  1. stirringthe mixture was stirred at room temperature for 4 h
  2. extractionThe mixture was extracted three times with ethyl acetate
  3. washthe combined organic layers were washed with brine
  4. dry with materialdried (magnesium sulfate)
  5. filtrationfiltered
  6. customevaporated
  7. custompurified by column chromatography
  8. washeluting with 25-50% ethyl acetate/hexanes

出典と根拠

ORDレコード
ord-a141a3563c134a8f8bb0a218f1afcc5e
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08188098B2

反応ノート

読み込み中…

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