関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Sodium Tartrate | HCID 9357 | — |
| 反応物 | 6-Methoxy-3,4-dihydro-1H-2-benzopyran-1-one | HCID 12401182 | — |
| 反応物 | Trimethylaluminum | HCID 16682925 | — |
| 反応物 | 4-(1,4-Dioxa-7-azaspiro[4.4]non-7-yl)-3-fluorophenylamine | HCID 21105431 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 68989883 | HCID 68989883 | — |
反応手順
A 2M solution of trimethylaluminum in toluene (14.9 mL) was added dropwise at 0° C. to a solution of 4-(1,4-dioxa-7-aza-spiro[4.4]non-7-yl)-3-fluorophenylamine (5.3 g) in methylene chloride (100.8 mL). The reaction mixture was stirred for 15 min at 0° C. and then for 30 min at room temperature. Then a solution of 6-methoxy-isochroman-1-one (3.8 g) in methylene chloride (40 mL) was added dropwise. The reaction mixture was stirred overnight at room temperature. Then saturated Rochelle salt solution was carefully added and the mixture was stirred for 1 h at room temperature. The aqueous phase was extracted several times with methylene chloride. The organic phases were combined, dried over sodium sulfate and the solvent was removed in vacuum. In this way the product was obtained with molecular weight 416.17 (C22H25FN2O5); MS (ESI): 417 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822495B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-a97c7772dc6149feb9d3501c939816d1 |
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| 出典メモ | uspto-grants-2014_09 |
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