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p-Toluenesulfonic acid → 2-((2-Chloroanilino)methyl)-2-imidazoline p-toluenesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 1,2-Ethanediamine, 4-methylbenzenesulfonate (1:?) | HCID 225030 | — |
| 反応物 | o-Chloroanilinoacetonitrile | HCID 12832554 | — |
| 反応物 | 2-((2-Chloroanilino)methyl)-2-imidazoline | HCID 13123534 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,2-Dichlorobenzene | HCID 7239 | — |
| 生成物 | 2-((2-Chloroanilino)methyl)-2-imidazoline p-toluenesulfonate | HCID 20529068 | — |
反応手順
The compound 2-((2-chloroanilino)methyl)-2-imidazoline p-toluenesulfonate was prepared using substantially the same procedure described above by heating a mixture of o-chloroanilinoacetonitrile (43.9 g), ethylenediamine p-toluenesulfonate (61.5 g) and 1,2-dichlorobenzene (198 ml). The p-toluenesulfonate salt was hydrolyzed to the free base, i.e., 2-((2-chloroanilino)methyl)-2-imidazoline by slurrying the p-toluenesulfonate salt in water, basifying the slurry and extracting the mixture with CH2Cl2. The methylene chloride was evaporated leaving 38.0 g of the free base. The free base was put in solution in isopropyl alcohol and acidified with hydrochloric acid in isopropyl alcohol which resulted in crystal formation.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04343810 |
| 出典データセット | uspto-grants-1982_08 |
| ORD ID | ord-ff23076f9cdd42e0951ae0a9c3896e80 |
| 出典メモ | uspto-grants-1982_08 |