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1-Cyclopropylpropan-2-one → (NE)-N-(1-cyclopropylpropan-2-ylidene)-2-methylpropane-2-sulfinamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Cyclopropylpropan-2-one | HCID 537025 | — |
| 反応物 | Tert-Butanesulfinamide | HCID 3382465 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (NE)-N-(1-cyclopropylpropan-2-ylidene)-2-methylpropane-2-sulfinamide | HCID 89424933 | — |
反応手順
A 25 mL round bottomed flask was charged with Ti(OEt)4 (technical grade, 0.37 mL, 1.4 mmol) and 1-cyclopropylpropan-2-one (79.0 mg, 0.81 mmol) in THF (1.45 mL), under an argon atmosphere. Then 2-methylpropane-2-sulfinamide (88.7 mg, 0.73 mmol) was added and the reaction mixture was heated to reflux overnight. After cooling to room temperature the reaction mixture was poured onto brine (1.7 mL), with rapid stirring. The resulting suspension was filtered through a pad of celite. The filtrate was concentrated under reduced pressure to afford crude 2-methyl-propane-2-sulfinic acid [2-cyclopropyl-1-methyl-eth-(E)-ylidene]-amide which was taken directly to the next step without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08658646B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-dd64737ef56e482fa2d953cc0235999b |
| 出典メモ | uspto-grants-2014_02 |