化工社化工社 化学情報印刷レポート · 研究参考用
1,3-Dichloro-2-isothiocyanatobenzene → N-(2,6-Dichlorophenyl)-3-[3-(trifluoromethyl)phenoxy]-1-azetidinecarbothioamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,3-Dichloro-2-isothiocyanatobenzene | HCID 123239 | — |
| 反応物 | 3-[3-(Trifluoromethyl)phenoxy]azetidine | HCID 11138538 | — |
| 反応物 | HCID 178418790 | HCID 178418790 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | N-(2,6-Dichlorophenyl)-3-[3-(trifluoromethyl)phenoxy]-1-azetidinecarbothioamide | HCID 15053384 | 90.2% |
反応手順
A solution of 0.04 mole of 3-[3-(trifluoromethyl) phenoxy]azetidine in 100 ml of absolute ethanol was stirred in a tap water bath while 8.16 g (0.04 mole) of 2,6-dichlorophenyl isothiocyanate was added all at once. The reaction was slightly exothermic and as the isothiocyanate began to dissolve, product began to precipitate. After stirring for 45 minutes the reaction mixture was heated on a steam bath to assure that all the isothiocyanate dissolved, and upon cooling, filtration yielded 15.2 g of white crystalline product. A portion of this material (7.9 g) was recrystallized from absolute ethanol to give 4.3 g of pure crystalline powder, m.p. 196°-197° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05068231 |
| 出典データセット | uspto-grants-1991_11 |
| ORD ID | ord-2889d763bd8c4d559d166dcd12d8d557 |
| 出典メモ | uspto-grants-1991_11 |