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Ethylenediamine → Ethyl 2-fluorocyclopropanecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylenediamine | HCID 3301 | — |
| 反応物 | Ethyl 1-chloro-2-fluorocyclopropanecarboxylate | HCID 15346054 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 2-fluorocyclopropanecarboxylate | HCID 10313150 | 81% |
反応手順
An internal glass tube was introduced into an autoclave and 0.5 g of ethyl 1-chloro-2-fluoro-1-cyclopropanecarboxylate (cis:trans=1.4:1), 0.5 ml of Raney nickel and 5 ml of ethanol were fed thereinto. Then 0.18 mg of 1,2-diaminoethane was further added and the mixture was stirred at room temperature under an elevated hydrogen gas atmosphere (10 kgf/cm2) for 48 hours. After the completion of the reaction, the catalyst was filtered off. Then the reaction mixture containing the title compound was analyzed by gas chromatography. As a result, it was found out that the reaction conversion rate was 95%, the yield was 81% and the cis:trans ratio was 0.3:1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05780669 |
| 出典データセット | uspto-grants-1998_07 |
| ORD ID | ord-5656af2acacb4db4b1e2b0c10c97e9a2 |
| 出典メモ | uspto-grants-1998_07 |