Diethyl-2-chloro-propionyl-malonate → Diethyl-2-[4'-(2",4"-dichloro-phenoxy)-phenoxy]-propionyl-malonate

HRID 1709101ノート

反応式

HRID 1709101 の反応式
[Na].[Cl:2][C:3]1[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:4]=1[O:5][C:6]1[CH:11]=[CH:10][C:9]([O-:12])=[CH:8][CH:7]=1.[CH2:18]([O:20][C:21](=[O:33])[CH:22]([C:28](=[O:32])[CH:29](Cl)[CH3:30])[C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH3:19]>CS(C)=O>[CH2:26]([O:25][C:23](=[O:24])[CH:22]([C:28](=[O:32])[CH:29]([O:12][C:9]1[CH:8]=[CH:7][C:6]([O:5][C:4]2[CH:13]=[CH:14][C:15]([Cl:17])=[CH:16][C:3]=2[Cl:2])=[CH:11][CH:10]=1)[CH3:30])[C:21]([O:20][CH2:18][CH3:19])=[O:33])[CH3:27]

参加物

4

反応物 2

HCID 19765057Diethyl-2-chloro-propionyl-malonateHCID 86744142Sodium 4-(2',4'-dichloro-phenoxy)-phenolate

生成物 1

HCID 23037017Diethyl-2-[4'-(2",4"-dichloro-phenoxy)-phenoxy]-propionyl-malonate収率 63.9%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
60 °C

実験手順

27.7 g of sodium-4-(2',4'-dichloro-phenoxy)-phenolate and 25.1 g of diethyl-2-chloro-propionyl-malonate are dissolved in 150 ml of dimethyl sulfoxide and the reaction mixture is stirred at 60° C. for 48 hours under stirring. The reaction mixture is filtered and the filtrate is evaporated. The residue is dissolved in 100 ml of benzene and washed successively with 100 ml of a saturated aqueous sodium hydrogen carbonate solution and water. The benzene solution is evaporated. Thus 30 g of the desired compound are obtained, yield 61%.

後処理

  1. stirringunder stirring
  2. filtrationThe reaction mixture is filtered
  3. customthe filtrate is evaporated
  4. dissolutionThe residue is dissolved in 100 ml of benzene
  5. washwashed successively with 100 ml of a saturated aqueous sodium hydrogen carbonate solution and water
  6. customThe benzene solution is evaporated

出典と根拠

ORDレコード
ord-41bffb4b3a5a4b44a31d7fde63e87897
出典データセット
uspto-grants-1990_08
特許番号
US04948420

反応ノート

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