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HRID 324415作成日:2026年10月26日
Boron trifluoride etherate → (+/-)-5-(7-Ethyl-9,10-dihydro-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-yl)-2,4(1H,3H)-pyrimidinedione
https://huagongshe.com/reaction/324415
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Boron trifluoride etherate | HCID 8000 | — |
| 反応物 | Triethylsilane | HCID 12052 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | (+/-)-4-(2,4-Bis(1,1-dimethylethoxy)pyrimidin-5-yl)-7-ethyl-2-methyl-9,10-dihydro-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-ol | HCID 70113732 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (+/-)-5-(7-Ethyl-9,10-dihydro-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-yl)-2,4(1H,3H)-pyrimidinedione | HCID 70114236 | — |
反応手順
A stirred solution of the product from step (i) (0.60 g) in dichloromethane (15 ml) was treated with triethylsilane (0.225 ml) and cooled to 0° C. Boron trifluoride etherate (0.65 ml) was added in four equal portions at 5 minute intervals and the reaction stirred at room temperature for 16 hours. The reaction was poured into saturated sodium bicarbonate solution (200 ml) and extracted with ethyl acetate. The extracts were dried (MgSO4) and evaporated to give a yellow solid which was purified by reverse phase chromatography eluting with 50% to 80% methanol in 0.1% aqueous ammonium acetate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06218376B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-81e57e3676454468b17fdd38b48e4ab2 |
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| 出典メモ | uspto-grants-2001_04 |
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