Potassium Carbonate → Ethyl 2-[4-(para-chlorobenzoyl)-phenoxy]-propionate

HRID 225116

反応式

HRID 225116 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:16])[C:9]2[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=2)=[CH:4][CH:3]=1.C([O-])([O-])=O.[K+].[K+].Br[CH:24]([CH3:30])[C:25]([O:27][CH2:28][CH3:29])=[O:26]>CC(CC(C)C)=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([C:9]2[CH:14]=[CH:13][C:12]([O:15][CH:24]([CH3:30])[C:25]([O:27][CH2:28][CH3:29])=[O:26])=[CH:11][CH:10]=2)=[O:16])=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 79040Ethyl 2-bromopropionateHCID 1235044-Hydroxy-4'-chlorobenzophenone

生成物 1

HCID 20143873Ethyl 2-[4-(para-chlorobenzoyl)-phenoxy]-propionate

試薬・触媒・溶媒 1

HCID 7909Methyl Isobutyl Ketone溶媒

実験手順

0.75 mole (175 g) of 4'-chloro-4-hydroxy-benzophenone, 1.5 l of methylisobutylketone, 0.975 mole (134 g) of K2CO3 and 0.8 mole (145 g) of ethyl 2-bromopropionate are placed in a 2-liter flask. The mixture is heated at reflux for 8 hours with vigorous agitation whereupon the reaction mixture is cooled and filtered on a Buchner funnel. The solvent is then evaporated under vacuum and the residue distilled; the desired ester is recovered at 198° to 201° C. under 0.1 mm of mercury. Yield 190 g (76%).

後処理

  1. temperatureThe mixture is heated
  2. temperatureat reflux for 8 hours with vigorous agitation whereupon the reaction mixture
  3. temperatureis cooled
  4. filtrationfiltered on a Buchner funnel
  5. customThe solvent is then evaporated under vacuum
  6. distillationthe residue distilled
  7. customthe desired ester is recovered at 198° to 201° C. under 0.1 mm of mercury

出典と根拠

ORDレコード
ord-9759be4baaca402c9204b1d5642af1fd
出典データセット
uspto-grants-1980_11
特許番号
US04235896

関連ノート

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