化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 6-Trifluoromethoxy-1-trifluoromethylsulphenylindazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfenyl chloride, trifluoro- | HCID 67900 | — |
| 反応物 | 6-(Trifluoromethoxy)-1H-indazole | HCID 13712997 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 6-Trifluoromethoxy-1-trifluoromethylsulphenylindazole | HCID 13713012 | — |
反応手順
20.2 g (0.1 mole) of 6-trifluoromethoxyindazole and 10.1 g (0.1 mole) of triethylamine in 125 ml of toluene are heated to 80° to 85° C., and 13.6 g (0.1 mole) of trifluoromethanesulphenyl chloride are then passed in the course of one hour and the mixture is stirred for a further hour at this temperature. After cooling, the precipitated triethylamine hydrochloride is filtered off with suction and rinsed with toluene. The filtrate, combined with the wash liquor, is washed twice with water. After drying (MgSO4) the volatile constituents are removed by distillation under a water pump vacuum. The oily crude product is purified by distillation under an oil pump vacuum. Boiling point 62°/0.05 mbar. Yield: 16.2 g (46% of theory).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04778511 |
| 出典データセット | uspto-grants-1988_10 |
| ORD ID | ord-ffd70e6dcf6542288e1094786099fbe2 |
| 出典メモ | uspto-grants-1988_10 |