Water → HCID 21186673、化合物

HRID 1384273ノート

反応式

HRID 1384273 の反応式
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

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 21186674HCID 21186674、化合物

生成物 1

HCID 21186673HCID 21186673、化合物収率 79.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-168ac60ef0c04aa989de80fa72b0a94a
出典データセット
uspto-grants-2001_07
特許番号
US06258829B1

反応ノート

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