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2-Chloro-N,N-diethyl-1,1,2-trifluoroethan-1-amine → 7-[2-(2-Thienyl)acetamido]-3-fluoro-3-cephem-4-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Chloro-N,N-diethyl-1,1,2-trifluoroethan-1-amine | HCID 136184 | — |
| 反応物 | p-Nitrobenzyl 7-[2-(2-thienyl)acetamido]-3-hydroxy-3-cephem-4-carboxylate | HCID 70559815 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 7-[2-(2-Thienyl)acetamido]-3-fluoro-3-cephem-4-carboxylic acid | HCID 70560081 | — |
反応手順
To a solution of 325 mg. (0.7 mmole) of p-nitrobenzyl 7-[2-(2-thienyl)acetamido]-3-hydroxy-3-cephem-4-carboxylate in 10 ml. of methylene chloride was slowly added an equivalent amount of N-(2-chloro-1,1,2-trifluoroethyl) diethylamine. The reaction mixture was heated for 30 minutes under gentle reflux and was then evaporated to dryness in vacuo. The residue was dissolved in a mixture of ethyl acetate-water and the organic layer was separated. The organic layer was washed with 5% hydrochloric acid, water and brine and was then dried. The dried reaction product solution was concentrated to a small volume and n-hexane was added to precipitate, p-nitrobenzyl 7-[2-(2-thienyl)acetamido]-3-fluoro-3-cephem-4-carboxylate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04260745 |
| 出典データセット | uspto-grants-1981_04 |
| ORD ID | ord-98fbd01fc10143498ca6389d234b97cc |
| 出典メモ | uspto-grants-1981_04 |