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Sodium Hydroxide → 6-Methyl-2-oxo-5-phenyl-1-[3-(trifluoromethyl)phenyl]-1,2-dihydropyridine-3-carboxylic acid

HRID 559819
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HRID 559819 반응식
[OH-].[Na+].[CH3:3][C:4]1[N:9]([C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[CH:11]=2)[C:8](=[O:20])[C:7]([C:21]([O:23]CC)=[O:22])=[CH:6][C:5]=1[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1>C1COCC1.CO.O>[CH3:3][C:4]1[N:9]([C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:17])([F:18])[F:19])[CH:11]=2)[C:8](=[O:20])[C:7]([C:21]([OH:23])=[O:22])=[CH:6][C:5]=1[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1
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참가 물질

6

반응물 2

HCID 14798Sodium HydroxideHCID 66725250Ethyl 6-methyl-2-oxo-5-phenyl-1-[3-(trifluoromethyl)phenyl]-1,2-dihydropyridine-3-carboxylate

생성물 1

HCID 667252216-Methyl-2-oxo-5-phenyl-1-[3-(trifluoromethyl)phenyl]-1,2-dihydropyridine-3-carboxylic acid수율 78.3%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매

실험 절차

Aqueous 2M sodium hydroxide solution (2.5 ml, 5.0 mmol) was added to a solution of ethyl 6-methyl-2-oxo-5-phenyl-1-[3-(trifluoromethyl)phenyl]-1,2-dihydropyridine-3-carboxylate (0.85 g, 2.12 mmol) in THF (5 ml), methanol (3 ml) and water (1 ml). The reaction mixture was stirred at room temperature for 2 h and then concentrated in vacuo. Acetonitrile (3 ml) was added to the residue and the solution was acidified using TFA. The resulting solid was collected by filtration, washed with water and acetone and air dried to give the title compound as white solid (0.62 g, 78%).

후처리

  1. concentrationconcentrated in vacuo
  2. additionAcetonitrile (3 ml) was added to the residue
  3. filtrationThe resulting solid was collected by filtration
  4. washwashed with water and acetone and air
  5. customdried

출처 및 근거

ORD 기록
ord-1ecde97683ea4582a15b89dc3dc05a58
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08063073B2

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