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5-chloro-N-methylpyridin-2-amine → 1,1-bis(phenylsulphonyl)-2-[N-(5-chloropyrid-2-yl)-N-methylamino]ethene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 5-chloro-N-methylpyridin-2-amine | HCID 3837024 | — |
| 反応物 | 1,1-Bis(phenylsulphonyl)-2-ethoxyethene | HCID 12400938 | — |
| 触媒 | Hydrochloric Acid | HCID 313 | — |
| 触媒 | 1,5-Diazabicyclo(4.3.0)non-5-ene | HCID 76349 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1,1-bis(phenylsulphonyl)-2-[N-(5-chloropyrid-2-yl)-N-methylamino]ethene | HCID 20207440 | — |
反応手順
A mixture of 5-chloro-2-(methylamino)pyridine (0.41 g), 2-ethoxy-1,1-bis(phenylsulphonyl)ethene and concentrated hydrochloric acid (1 drop) in toluene (20 ml) was heated at reflux for 4 hours and then the mixture was treated with 1,5-diazabicyclo[4.3.0]-non-5-ene (3 drops) and heated at reflux for 18 hours. The reaction mixture was cooled and concentrated in vacuo to give an oil which was triturated with ethanol to give a brown solid which was recrystallised from toluene to give 1,1-bis(phenylsulphonyl)-2-[N-(5-chloropyrid-2-yl)-N-methylamino]ethene (0.2 g), mp. 205°-206° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04659727 |
| 出典データセット | uspto-grants-1987_04 |
| ORD ID | ord-b3a9fe616479454fa1f454e11bde5baa |
| 出典メモ | uspto-grants-1987_04 |