1,2-Dichloroethane → 1,1-Cyclopropanedicarboxylic acid, 1,1-dimethyl ester

HRID 991262

反応式

HRID 991262 の反応式
Cl[CH2:2][CH2:3]Cl.CC(CC(O)CO)C.C(=O)([O-])[O-].[K+].[K+].[C:19]([O:26][CH3:27])(=[O:25])[CH2:20][C:21]([O:23][CH3:24])=[O:22]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.O>[C:20]1([C:19]([O:26][CH3:27])=[O:25])([C:21]([O:23][CH3:24])=[O:22])[CH2:3][CH2:2]1

参加物

7

反応物 4

HCID 111,2-Dichloroethane2 回HCID 7943Dimethyl malonateHCID 11430Potassium CarbonateHCID 911714-Methylpentane-1,2-diol

生成物 1

HCID 27695391,1-Cyclopropanedicarboxylic acid, 1,1-dimethyl ester収率 95%

試薬・触媒・溶媒 2

HCID 74236Tetrabutylammonium Bromide触媒HCID 962Water溶媒

実験手順

296.9 g of 1,2-dichloroethane (3 mol), 15 g of polyethylene glycol dimethyl ether (mean molar mass 500 g/mol) and 177.1 g of potassium carbonate (1.265 mol) were initially introduced, and the reaction mixture was heated until the 1,2-dichloroethane refluxes. 125.5 g of dimethyl malonate (0.95 mol) and 1.25 g of tetrabutylammonium bromide (3.88 mmol) were then added at the boil. The mixture was stirred using a paddle stirrer for 6 hours. Water formed during the reaction was removed by azeotropic distillation with 1,2-dichloroethane throughout the reaction. Further work-up was carried out analogously to Comparative Example 2. The yield was 95%.

後処理

  1. customfor 6 hours
  2. customwas removed by azeotropic distillation with 1,2-dichloroethane throughout the reaction

出典と根拠

ORDレコード
ord-52cac8cab06c43de8be40cf7c82cf8d9
出典データセット
uspto-grants-2002_10
特許番号
US06462224B2

関連ノート

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