Carbon Dioxide → HCID 68133938、化合物

HRID 1605644

反応式

HRID 1605644 の反応式
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[C:6]([F:16])[CH:5]=1)(=O)[CH3:2].[CH2:17]([O:19]C(=O)/C=C(/OCC)\C)[CH3:18].Cl.[C:29](=O)=O>CN(C)C=O>[F:16][C:6]1[CH:5]=[C:4](/[C:1](/[CH3:29])=[CH:2]/[C:17](=[O:19])[CH3:18])[CH:9]=[CH:8][C:7]=1[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

6

反応物 4

HCID 280Carbon DioxideHCID 313Hydrochloric AcidHCID 5354173Ethyl (2E)-3-ethoxy-2-butenoateHCID 64519181-(2-Fluoro(1,1'-biphenyl)-4-yl)ethan-1-one

生成物 1

HCID 68133938HCID 68133938、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

72.8 Gm (0.649 mol) of potassium tert.butylate were added all at once to a slution of 97.0 gm (0.453 mol) of 4-acetyl-2-fluoro-biphenyl and 103.0 gm (0.651 mol) of (E)-3-ethoxy-crotonic acid ethyl ester in 1 liter of anhydrous dimethylformamide, whereby the temperature of the mixture rose spontaneously from 20°C to 38°C and its color turned intensely red. The reaction mixture was stirred for one hour while maintaining an internal temperature of 32° to 35°C, and then, while the mixture was still warm, 200 ml of concentrated hydrochloric acid were added dropwise thereto, and the resulting mixture was heated for 30 minutes at 90°-100°C. After the evolution of carbon dioxide had ceased, the cooled mixture was stirred into one liter of ice water, and the yellowish precipitate formed thereby was filtered off, thoroughly washed with water and recrystallized, in the presence of activated charcoal, once from methanol and twice from diisopropyl ether. 75.0 gm (65% of theory) of the fallow crystalline compound, m.p. 103°C, of the formula ##SPC21##

後処理

  1. customrose spontaneously from 20°C to 38°C
  2. temperaturewhile maintaining an internal temperature of 32° to 35°C
  3. temperaturewhile the mixture was still warm
  4. temperaturethe resulting mixture was heated for 30 minutes at 90°-100°C
  5. customthe yellowish precipitate formed
  6. filtrationthereby was filtered off
  7. washthoroughly washed with water
  8. customrecrystallized, in the presence of activated charcoal, once from methanol and twice from diisopropyl ether

出典と根拠

ORDレコード
ord-5184725057694ede9a51c1a537f6831b
出典データセット
uspto-grants-1976_04
特許番号
US03950427

関連ノート

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