関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-(Trifluoromethyl)aniline | HCID 7375 | — |
| 反応物 | Propargyl bromide | HCID 7842 | — |
| 生成物 | Benzenamine, N-2-propyn-1-yl-3-(trifluoromethyl)- | HCID 10488213 | 34.8% |
反応手順
A mixture of 3-trifluoromethylaniline (30 g) ad propargyl bromide (12 g) was stirred at 80° C. for 3 hours, followed by filtration of the reaction mixture. The filtrate was subjected to column chromatography to give N-propargyl-3-trifluoromethylaniline (7 g). A solution of N-propargyl-3-trifluoromethylaniline thus obtained (5.1 g) and ethoxycarbonyl isothiocyalate (3.7 g) in tetrahydrofuran (100 ml) was stirred at room temperature for 8 hours, and the solvent was removed under reduced pressure. The concentrated residue was extracted with chloroform (200 ml), washed with water and dried over anhydrous magnesium sulfate. After removal of the solvent, the residue was subjected to column chromatography to give 5.7 g of 2 -ethoxycarbonylimino-3-(3-trifluoromethylphenyl)-5-methylenethiazolidine (Compound (i)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05244863 |
|---|
| 出典データセット | uspto-grants-1993_09 |
|---|
| ORD ID | ord-d71d3da489d640ec9419ef589183bfc0 |
|---|
| 出典メモ | uspto-grants-1993_09 |
|---|