関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1,3-Difluoro-2-propanol | HCID 67985 | — |
| 反応物 | Methyl 5,6-Dichloronicotinate | HCID 2782166 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 5-chloro-6-[(1,3-difluoropropan-2-yl)oxy]nicotinate | HCID 67363966 | 80.7% |
反応手順
Methyl 5,6-dichloronicotinate (1.5 g) and 60% sodium hydride (640 mg) were dissolved in THF (45 mL). 1,3-Difluoropropan-2-ol (1.5 g) was added thereto at 0° C., followed by stirring at 0° C. for 3 hours, and the reaction solution was quenched with aqueous NH4Cl. After extraction with EtOAc, the organic layer was dried over MgSO4 and then filtered, and the desiccant was removed. The vehicle was evaporated under reduced pressure, followed by purification by silica gel column chromatography (hexane:AcOEt=100:0 to 50:50) to obtain methyl 5-chloro-6-[(1,3-difluoropropan-2-yl)oxy]nicotinate (1.56 g) as a colorless liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08193378B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-6d3346eb5732435ab3e1c1b3e3aff310 |
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| 出典メモ | uspto-grants-2012_06 |
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