関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3-(2,6-Dichloro-pyrimidin-4-yl)-8-oxa-3-aza-bicyclo[3.2.1]octane | HCID 86665879 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 178517808 | HCID 178517808 | 221.4% |
反応手順
In three 2-5 mL microwave vials was each placed 3-(2,6-dichloropyrimidin-4-yl)-8-oxa-3-azabicyclo[3.2.1]octane (9, 100 mg, 0.384 mmol) in THF (2 ml). A 1N solution of sodium hydroxide (2 ml, 2.000 mmol) was added to each vial. The reaction was heated under microwave irradiation at 150° C. for 30 min. The contents of the three microwave vials were combined, 6 mL 2N HCl was added to acidify (pH˜3). Silica gel was added and the mixture was concentrate purify by silica gel chromatography, using a gradient (0-15%) of MeOH in dichloromethane to give 205 mg (0.85 mmol, 74%) of the title compound as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08835429B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-2d7f2707bc70492490fb745c634e527b |
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| 出典メモ | uspto-grants-2014_09 |
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