関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 5H-Dibenzo[a,d]cyclohepten-5-one | HCID 16679 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 5-Bromo-2,4-bis(1,1-dimethylethoxy)pyrimidine | HCID 818851 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-(2,4-bis(1,1-dimethylethoxy)pyrimidin-5-yl)-5H-dibenzo[a,d]cyclohepten-5-ol | HCID 21250882 | — |
反応手順
To a solution of the product of step (i) (50 g) in dry tetrahydrofuran (11) at −78° C. was added n-butyllithium (69 ml of a 2.5 M solution in hexanes) dropwise. After 0.5 hours a solution of 5H-dibenzo[a,d]cyclohepten-5-one (44 g) in tetrahydrofuran (100 ml) was added. The reaction mixture was stirred at −78° C. for three hours and then allowed to warm to room temperature overnight. Saturated aqueous ammonium chloride solution (400 ml) was added and the mixture extracted with ethyl acetate. The organic solution was dried (MgSO4) and evaporated under reduced pressure to give the crude 5-[2,4-bis[1,1-dimethylethoxy]pyrimidin-5-yl]-5H-dibenzo[a,d]cyclohepten-5-ol which was used directly.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06200981B1 |
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| 出典データセット | uspto-grants-2001_03 |
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| ORD ID | ord-b67e701fdc6a4dd4ae5231942ef25189 |
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| 出典メモ | uspto-grants-2001_03 |
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