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Triethylamine → 3-Methyl-2-(4'-trichloromethylbenzoyl methylene)-benzothiazoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-(Trichloromethyl)benzoyl chloride | HCID 84660 | — |
| 反応物 | Benzothiazolium, 2,3-dimethyl-, 4-methylbenzenesulfonate (1:1) | HCID 102307 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3-Methyl-2-(4'-trichloromethylbenzoyl methylene)-benzothiazoline | HCID 53967611 | — |
反応手順
2,3-dimethylbenzothiazolinium-p-toluene sulphonate (10 g) was slurried in dry toluene (50 ml) and cooled to 5 degC. A solution of 4-trichloromethylbenzoyl chloride (8.9 g) in dry toluene (10 ml) was added dropwise to the stirred slurry over a period of 30 minutes, maintaining the temperature at 10-15 degC. A solution of triethylamine (7 ml) in dry toluene (10 ml) was then added dropwise over a period of 30 minutes, the temperature again being maintained at 10-15 degC. The reaction mixture was stirred for two hours at room temperature. The solid product was filtered off, reslurried in methanol and recrystallised from a 3/1 chloroform/methanol solution.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05141841 |
| 出典データセット | uspto-grants-1992_08 |
| ORD ID | ord-127389f293034698a8b786a9e8623cc2 |
| 出典メモ | uspto-grants-1992_08 |