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Ammonium Chloride → HCID 67398402, 화합물

HRID 70709
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HRID 70709 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 5049666Sodium triacetoxyborohydrideHCID 67399727HCID 67399727, 화합물

생성물 1

HCID 67398402HCID 67398402, 화합물수율 36.1%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-b57227c17d40432ea13c02db8d4882f1
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08822503B2

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