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Water → HCID 67009484, 화합물

HRID 2194544
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HRID 2194544 반응식
[CH3:1][N:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([C:12]([F:15])([F:14])[F:13])[N:10]=2)[CH:5]=[C:4]([C:16]([O:18]CC)=[O:17])[C:3]1=[O:21].O.[OH-].[Li+].O.C(=O)([O-])O.[Na+]>O1CCOCC1>[CH3:1][N:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([C:12]([F:15])([F:13])[F:14])[N:10]=2)[CH:5]=[C:4]([C:16]([OH:18])=[O:17])[C:3]1=[O:21]
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참가 물질

6

반응물 4

HCID 962WaterHCID 168937Lithium hydroxide, monohydrateHCID 516892Sodium BicarbonateHCID 67009647HCID 67009647, 화합물

생성물 1

HCID 67009484HCID 67009484, 화합물수율 91.4%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

1.24 g (4.1 mmol) of ethyl 1-methyl-2-oxo-7-(trifluoromethyl)-1,2-dihydro-1,8-naphthyridine-3-carboxylate was dissolved in 1,4-dioxane (50 mL), and 0.35 g (8.3 mmol) of lithium hydroxide monohydrate and 10 mL of water were added thereto at room temperature. The resulting mixture was stirred overnight at room temperature. The reaction mixture was poured into an aqueous solution of sodium hydrogen carbonate, and the mixture was washed with ethyl acetate. The aqueous phase was acidified with citric acid, and the mixture was extracted with ethyl acetate. The organic phase was washed with water, dried, and concentrated. The residue was washed with normal-hexane, and thus 1.02 g of the title compound was obtained as colorless crystals (yield: 91%).

후처리

  1. customat room temperature
  2. washthe mixture was washed with ethyl acetate
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic phase was washed with water
  5. customdried
  6. concentrationconcentrated
  7. washThe residue was washed with normal-hexane

출처 및 근거

ORD 기록
ord-090e96e839d441acb05c7a297035cf9e
출처 데이터셋
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08334236B2

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