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Ethyl Acetate → N-(dibenzo[b,d]furan-2-ylmethylene)-2-methylpropane-2-sulfinamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Dibenzo(b,d)furan-2-carboxaldehyde | HCID 220843 | — |
| 反応物 | Tert-Butanesulfinamide | HCID 3382465 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | N-(dibenzo[b,d]furan-2-ylmethylene)-2-methylpropane-2-sulfinamide | HCID 86695630 | — |
反応手順
A mixture of commercially available dibenzo[b,d]furan-2-carbaldehyde (1.992 g; 10.20 mmol), titanium(IV) ethoxide Ti(OEt)4 (3.98 ml; 19.00 mmol), and 2-methylpropane-2-sulfinamide (1.150 g; 9.49 mmol) in anh. THF (18 ml) was stirred at rt, under nitrogen, for 4 h. AcOEt and brine were added, and the organic layer was further washed with brine, dried over anh. MgSO4, filtered, and concentrated to dryness under reduced pressure. Purification by FC (DCM) afforded N-(dibenzo[b,d]furan-2-ylmethylene)-2-methylpropane-2-sulfinamide as a pale yellow solid. LC-MS (conditions A): tR=0.96 min.; [M+H]+: 300.33 g/mol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09242970B2 |
| 出典データセット | uspto-grants-2016_01 |
| ORD ID | ord-52acc40b5af041ff86e04ebb99c8d6e1 |
| 出典メモ | uspto-grants-2016_01 |