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Hydrochloric Acid → 6'-Bromospiro[cyclobutane-1,2'-inden]-1'(3'H)-imine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | N-(5'-Bromospiro[cyclobutane-1,2'-indene]-3'(1'H)-ylidene)-2-methylpropane-2-sulfinamide | HCID 67979440 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 6'-Bromospiro[cyclobutane-1,2'-inden]-1'(3'H)-imine | HCID 67979393 | — |
反応手順
Hydrochloric acid (4M in 1,4-dioxane, 14.89 mL, 59.55 mmol) was added to a solution of N-(5′-bromospiro[cyclobutane-1,2′-indene]-3′(1′H)-ylidene)-2-methylpropane-2-sulfinamide (Example 54 Step 1, 2.11 g, 5.96 mmol) in anhydrous 1,4-dioxane (60 mL), and the resulting mixture was stirred under an argon atmosphere for 3 h. Et2O (4 mL) was added and the precipitate was filtered off and washed with Et2O, then partitioned between DCM (100 mL), and sat. aq. NaHCO3 (100 mL). The phases were separated and the organic layer concentrated to afford the title compound that was used as such without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08415483B2 |
| 出典データセット | uspto-grants-2013_04 |
| ORD ID | ord-6fbc229fbab646ab9e063be46861ca16 |
| 出典メモ | uspto-grants-2013_04 |