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Sodium Bicarbonate → N-(1,4-dioxaspiro[4.5]dec-8-ylidene)-2-methylpropane-2-sulfinamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1,4-Dioxaspiro[4.5]decan-8-one | HCID 567415 | — |
| 反応物 | Tert-Butanesulfinamide | HCID 3382465 | — |
| 触媒 | Titanium tetraethoxide | HCID 76524 | — |
| 生成物 | N-(1,4-dioxaspiro[4.5]dec-8-ylidene)-2-methylpropane-2-sulfinamide | HCID 59733754 | 45.8% |
反応手順
An oven dried round-bottom flask was cooled to room temperature by flushing with N2(g) for 30 min. 1,4-Dioxa-spiro[4.5]decan-8-one (1.35 g, 8.66 mmol) (dissolved in 12 mL THF), 2-Methyl-propane-2-sulfinic acid amide (1.0 g, 8.25 mmol) (dissolved in THF), and titanium(IV) ethoxide (3.77 g, 16.50 mmol) were added. The reaction was stirred for 4 h at room temperature. To the mixture was added 15 mL saturated NaHCO3 followed by filtration and an EtOAc rinse. The organic layer was dried with MgSO4, filtered and concentrated under reduced pressure yielding 0.98 g of Compound 15.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07385085B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-daa05a7ddeb148df9d3a671b4d156bfb |
| 出典メモ | uspto-grants-2008_06 |