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Sodium Chloride → Cyclopropanecarboxylic acid, 3-(2,2-dichloroethenyl)-2,2-dimethyl-, ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | 2,3-Dihydro-1-methyl-1H-phosphole 1-oxide | HCID 70104 | — |
| 反応物 | Ethyl 2-(2,2-dichlorovinyl)-3,3-dimethyl-1-ethoxycarbonylcyclopropanecarboxylate | HCID 14914133 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Cyclopropanecarboxylic acid, 3-(2,2-dichloroethenyl)-2,2-dimethyl-, ethyl ester | HCID 101094 | 90% |
反応手順
30 g (0.1 mol) of 2,2-dimethyl-3-(2',2'-dichlorovinyl)-cyclopropane-1,1-dicarboxylic acid diethyl ester, 50 ml of 1-oxo-1-methyl-phospholine, 6 g of sodium chloride and 4 ml of water were heated to 175° C. for 9 hours. The mixture was then cooled, poured into 150 ml of water and extracted with petroleum ether. After drying with MgSO4, the mixture was fractionally distilled. 21.3 g (=90% of theory) of 2,2-dimethyl-3-(2',2'-dichlorovinyl)-cyclopropane-1-carboxylic acid ethyl ester of boiling point 65°-75° C./0.1 mm Hg were obtained. 49.7 g of 1-oxo-1-methyl-phospholine of boiling point 75°-77° C./0.15 mm Hg were recovered by fractional distillation of the aqueous phase.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04276225 |
| 出典データセット | uspto-grants-1981_06 |
| ORD ID | ord-fc7aa8eebf7d4aa594b72af9cf0a8909 |
| 出典メモ | uspto-grants-1981_06 |