関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Tert-Butanesulfinamide | HCID 3382465 | — |
| 反応物 | 3-Oxetanone | HCID 15024254 | — |
| 触媒 | HCID 178477244 | HCID 178477244 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | 2-Methyl-N-(oxetan-3-ylidene)propane-2-sulfinamide | HCID 46839995 | — |
反応手順
To a 250 mL round-bottomed flask was added 2-methylpropane-2-sulfinamide (3.36 g, 27.8 mmol) followed by tetraethoxytitanium (11.64 ml, 55.5 mmol) to a tetrahydrofuran (69.4 ml) solution of oxetan-3-one (2 g, 27.8 mmol) at room temperature. The mixture was stirred at 50° C. for 5 hours, cooled and poured into brine. The suspension was filtered through a pad of diatomaceous earth eluting with ethyl acetate. The organics were combined, dried with sodium sulfate, filtered and concentrated under vacuum. The residue was purified by regular phase flash column chromatography to give the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09302989B2 |
|---|
| 出典データセット | uspto-grants-2016_04 |
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| ORD ID | ord-3d453ee755554741a9d6bc4cb6c12527 |
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| 出典メモ | uspto-grants-2016_04 |
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