Water → HCID 21186673, 화합물

HRID 1384273노트

반응식

HRID 1384273 반응식
C([O:4][CH:5]1[C:11]2=[N:12][C:13]([CH3:21])=[C:14]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH:15]=[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6]1)(=O)C.C(=O)([O-])[O-].[K+].[K+].O.C(OCC)(=O)C>C(O)C>[OH:4][CH:5]1[C:11]2=[N:12][C:13]([CH3:21])=[C:14]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH:15]=[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6]1

참가 물질

6

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 21186674HCID 21186674, 화합물

생성물 1

HCID 21186673HCID 21186673, 화합물수율 79.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Ethyl 9-acetoxy-2-methyl-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridine-3-carboxylate (4.90 g, 16.81 mmol) was dissolved in ethanol (30 ml), and the solution was mixed with potassium carbonate (3.29 g) and stirred at from 0° C. to room temperature for 24 hours. There action solution was mixed with water and ethyl acetate, and the thus precipitated crystals were filtered. The resulting filtrate was extracted with ethyl acetate, and the thus obtained organic layer was washed with water and saturated brine in that order and dried over anhydrous sodium sulfate. By evaporating the solvent under reduced pressure, the title compound (3.31 g, 79.9%) was obtained as pale yellow amorphous.

후처리

  1. filtrationthe thus precipitated crystals were filtered
  2. extractionThe resulting filtrate was extracted with ethyl acetate
  3. washthe thus obtained organic layer was washed with water and saturated brine in that order
  4. dry with materialdried over anhydrous sodium sulfate
  5. customBy evaporating the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-168ac60ef0c04aa989de80fa72b0a94a
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06258829B1

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