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Hydrochloric Acid → HCID 178418429、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | 3-cyano-4-trifluoromethylsulfenyl-5-(N-trifluoroacetylamino)pyrazole | HCID 178418360 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 178418429 | HCID 178418429 | 87.6% |
反応手順
The product of Step E (55 g, 181 mmoles) was dissolved in methanol. 100 ml of ammonium hydroxide were added, the solution was refluxed for 3 hours and then stirred at room temperature for 15 hours. The methanolic solution was brought to pH7 using concentrated aqueous hydrochloric acid and diluted with ethyl acetate. The organic layer was washed several times with water and brine, dried over MgSO4 and concentrated to dryness to give an oily brown residue which was recrystallized from methyl tert-butyl ether to afford 33 g of the title compound, m.p. around 187° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05726324 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-519d1ed0c254438c8f86070fac54bfc1 |
| 出典メモ | uspto-grants-1998_03 |