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Ammonium Chloride → HCID 67398402、化合物

HRID 70709
ノート
印刷プレビュー

反応式

HRID 70709 の反応式
C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[CH:15]1([S:18][C:19]2[CH:24]=[CH:23][C:22]([C:25]([C:27]3[NH:32][C:31](=[O:33])[C:30]([C:34]([F:37])([F:36])[F:35])=[CH:29][CH:28]=3)=[O:26])=[CH:21][CH:20]=2)[CH2:17][CH2:16]1.[Cl-].[NH4+]>C(Cl)(Cl)Cl>[CH:15]1([S:18][C:19]2[CH:24]=[CH:23][C:22]([CH:25]([OH:26])[C:27]3[NH:32][C:31](=[O:33])[C:30]([C:34]([F:36])([F:35])[F:37])=[CH:29][CH:28]=3)=[CH:21][CH:20]=2)[CH2:17][CH2:16]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 5049666Sodium triacetoxyborohydrideHCID 67399727HCID 67399727、化合物

生成物 1

HCID 67398402HCID 67398402、化合物収率 36.1%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

Sodium triacetoxyborohydride (125 mg) was added to a solution of 6-{[4-(cyclopropylsulfanyl)phenyl]carbonyl}-3-(trifluoromethyl)pyridin-2(1H)-one (110 mg) in chloroform (3 mL), and the mixture was stirred at room temperature overnight. An ammonium chloride solution was added to the reaction solution, followed by extraction with chloroform. The organic layer was dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate only) to give 6-{[4-(cyclopropylsulfanyl)phenyl](hydroxy)methyl}-3-(trifluoromethyl)pyridin-2(1H)-one (40 mg, 36%).

後処理

  1. extractionfollowed by extraction with chloroform
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. customThe solvent was evaporated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (ethyl acetate only)

出典と根拠

ORDレコード
ord-b57227c17d40432ea13c02db8d4882f1
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822503B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート