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Ethanol → Ethyl 1,2,3,4-tetrahydro-3-(1-methyl-1H-imidazol-2-yl)-4-oxo-2-[4-(trifluoromethyl)phenyl]-5-quinolinecarboxylate

HRID 1968048
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HRID 1968048 반응식
[F:1][C:2]([F:22])([F:21])[C:3]1[CH:20]=[CH:19][C:6](/[CH:7]=[N:8]/[C:9]2[CH:17]=[CH:16][CH:15]=[C:14]3[C:10]=2[CH2:11][O:12][C:13]3=[O:18])=[CH:5][CH:4]=1.[CH3:23][N:24]1[CH:28]=[CH:27][N:26]=[C:25]1[CH:29]=O.[O-:31][CH2:32][CH3:33].[Na+].C(O)C>C(OCC)(=O)CC>[CH3:23][N:24]1[CH:28]=[CH:27][N:26]=[C:25]1[CH:29]1[C:11](=[O:12])[C:10]2[C:14]([C:13]([O:31][CH2:32][CH3:33])=[O:18])=[CH:15][CH:16]=[CH:17][C:9]=2[NH:8][CH:7]1[C:6]1[CH:5]=[CH:4][C:3]([C:2]([F:21])([F:1])[F:22])=[CH:20][CH:19]=1
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참가 물질

6

반응물 4

HCID 702EthanolHCID 1395751-Methyl-2-imidazolecarboxaldehydeHCID 2723922Sodium ethoxideHCID 178519072HCID 178519072, 화합물

생성물 1

HCID 67260485Ethyl 1,2,3,4-tetrahydro-3-(1-methyl-1H-imidazol-2-yl)-4-oxo-2-[4-(trifluoromethyl)phenyl]-5-quinolinecarboxylate수율 8%

시약·촉매·용매 1

HCID 7749
Ethyl Propionate
용매

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온도
0 °C

실험 절차

A mixture of (E)-4-(4-(trifluoromethyl)benzylideneamino)isobenzofuran-1(3H)-one (1 g, 3.28 mmol) and N-methyl-2-imidazolecarbaldehyde (400 mg, 3.61 mmol) in ethyl propionate (40 mL) was cooled to 0° C. Then a solution of sodium ethoxide in ethanol (sodium (31 mg, 13.1 mmol) in ethanol (10 mL)) was added dropwise. After the addition, the mixture was stirred at room temperature for 2 hr. The mixture was quenched with water (10 mL) and solvent was removed in vacuum. The residue was dissolved in water, and then extracted with ethyl acetate (100 mL×4). The combined organic layers were washed with brine, dried over anhydrous sodium sulfate, and concentrated to give crude product. The crude product was purified by chromatography (silica gel, petroleum ether/ethyl acetate=1:1) to give the title compound (150 mg, yield 8%). LC-MS (ESI) m/z: 444 (M+1)+.

후처리

  1. additionAfter the addition
  2. customThe mixture was quenched with water (10 mL) and solvent
  3. customwas removed in vacuum
  4. dissolutionThe residue was dissolved in water
  5. extractionextracted with ethyl acetate (100 mL×4)
  6. washThe combined organic layers were washed with brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated
  9. customto give crude product
  10. customThe crude product was purified by chromatography (silica gel, petroleum ether/ethyl acetate=1:1)

출처 및 근거

ORD 기록
ord-302172e3701e4cc192fe46b188c5c6d1
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08420650B2

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