Benzene → (2,4-Dimethyl-phenyl)-(4-fluoro-phenyl)-methanone

HRID 1262721ノート

反応式

HRID 1262721 の反応式
Cl[C:2]1[CH:17]=[CH:16][C:5]([C:6]([C:8]2[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][C:9]=2[CH3:15])=[O:7])=[CH:4][CH:3]=1.[F-:18].[Cs+].CN1CCCC1=O.C1C=CC=CC=1>O>[F:18][C:2]1[CH:17]=[CH:16][C:5]([C:6]([C:8]2[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][C:9]=2[CH3:15])=[O:7])=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 241BenzeneHCID 13387N-methyl-2-pyrrolidoneHCID 25953Cesium fluorideHCID 6105854-Chloro-2',4'-dimethylbenzophenone

生成物 1

HCID 10242880(2,4-Dimethyl-phenyl)-(4-fluoro-phenyl)-methanone収率 78%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a mixture of 12.2 g (0.05 mols) of 4-chloro-2',4'-dimethylbenzophenone, 12.1 g (0.08 mols) of cesium fluoride and 20 g of N-methylpyrrolidone were 5 ml of benzene added and water in the reaction system was removed together with benzene by azeotropy. The reaction was carried out under nitrogen atmosphere under reflux by heating while stirring for 15 hours. After cooling, the reaction product obtained was poured into 100 ml of water and then, extracted with 50 ml of diethyl ether and further with 50 ml of ether. The extracts together were dried and distilled and thus, 8.9 g of 4-fluoro-2',4'-dimethylbenzophenone were obtained.

後処理

  1. additionadded
  2. customwater in the reaction system was removed together with benzene by azeotropy
  3. temperatureunder reflux
  4. temperatureby heating
  5. temperatureAfter cooling
  6. customthe reaction product obtained
  7. extractionextracted with 50 ml of diethyl ether and further with 50 ml of ether
  8. customThe extracts together were dried
  9. distillationdistilled

出典と根拠

ORDレコード
ord-88f76edc44844a389177ddba49135135
出典データセット
uspto-grants-1984_06
特許番号
US04453009

反応ノート

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