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Methyl Isocyanate → 1-(N-methylamino)carbonyl-4-(2,3,4,5,6-pentafluorophenoxy)-4-phenylpiperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl Isocyanate | HCID 12228 | — |
| 反応物 | 4-(2,3,4,5,6-Pentafluorophenoxy)-4-phenylpiperidine | HCID 14649978 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 1-(N-methylamino)carbonyl-4-(2,3,4,5,6-pentafluorophenoxy)-4-phenylpiperidine | HCID 14649980 | 69% |
反応手順
A solution of 5.0 g of 4-(2,3,4,5,6-pentafluorophenoxy)-4-phenylpiperidine in 50 ml of benzene was treated with a solution of 0.9 g of methyl isocyanate in 20 ml of benzene over a period of ten minutes. The reaction mixture was then stirred at ambient temperature for two hours. Evaporate of the volatiles afforded a solid which was purified by means of high pressure liquid chromatography (silica gel; elution with 50% ethyl acetate/dichloromethane) to yield 4.0 g (69%) of 1-(N-methylamino)carbonyl-4-(2,3,4,5,6-pentafluorophenoxy)-4-phenylpiperidine, m.p. 87°-89° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04853384 |
| 出典データセット | uspto-grants-1989_08 |
| ORD ID | ord-32ba7944d52a49e9ace3e7b2cd5c9a43 |
| 出典メモ | uspto-grants-1989_08 |