関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 4-(Chlorosulfonyl)phenyl acetate | HCID 12925710 | — |
| 反応物 | Alpha-Oximino-2-Thienylacetonitrile | HCID 73667355 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | alpha-(4-Acetoxybenzenesulfonyloxyimino)thien-2-ylacetonitrile | HCID 54491580 | 53.5% |
反応手順
200 mg of 4-dimethylaminopyridine and 6.2 g (0.08 mole) of pyridine are added to a solution of 12 g (0.08 mole) of α-hydroxyiminothien-2-ylacetonitrile (3b) in 75 ml of tetrahydrofuran. With cooling to 0° C., a solution of 18.5 g (0.08 mole) of 4-acetoxybenzenesulfonyl chloride (3a) in 30 ml of tetrahydrofuran is added dropwise. The reaction mixture is stirred for 16 hours at room temperature, and 100 ml of diethyl ether are subsequently added. The precipitated salts are removed by filtration and the solution is concentrated by evaporation. The residual crude product is recrystallised from hexane/ethyl acetate, affording 15 g of crystals with a melting point of 114°-115° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04736055 |
|---|
| 出典データセット | uspto-grants-1988_04 |
|---|
| ORD ID | ord-6e35bdfa6f57408fb75bc914e9662299 |
|---|
| 出典メモ | uspto-grants-1988_04 |
|---|
