関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Chloro-1,1-diethoxyethane | HCID 12128 | — |
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 反応物 | 3,4,4-Trifluoro-3-butenyl dithiocarbamate | HCID 11298598 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Thiazole, 2-[(3,4,4-trifluoro-3-butenyl)thio]- | HCID 11447455 | — |
反応手順
3 g (14.9 mmol) of 3,4,4-trifluoro-3-butenyl dithiocarbamate in 15 ml of glacial acetic acid are admixed with 2.3 g (15.1 mmol) of chloroacetaldehyde diethyl acetal and 40 mg of p-toluenesulphonic acid monohydrate. The mixture is stirred at 95° C. for 1.5 h and, after cooling to room temperature, is then concentrated by evaporation under reduced pressure. The evaporation residue is taken up in dichloromethane and washed with 1 N sodium hydroxide solution, and the organic phase is removed, dried over Na2SO4 and concentrated by evaporation under reduced pressure. 2.8 g (81.5% of theory; purity by GC/MS: 97.7 area %) of an oil are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07078527B2 |
|---|
| 出典データセット | uspto-grants-2006_07 |
|---|
| ORD ID | ord-ee4b179577564cf2a3db73ccda4e6fac |
|---|
| 出典メモ | uspto-grants-2006_07 |
|---|