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phosphorous acid, trisodium salt → 5-Cyclopropoxy-2-methylpyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | phosphorous acid, trisodium salt | HCID 134681 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-Methyl-5-[1-(phenylsulfonyl)cyclopropoxy]pyridine | HCID 66598322 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-Cyclopropoxy-2-methylpyridine | HCID 58520641 | 86% |
反応手順
2-Methyl-5-(1-(phenylsulfonyl)cyclopropoxy)pyridine (540 mg, 1.87 mmol) was dissolved in methanol (5.5 mL), and sodium phosphite (671 mg, 5.598 mmol) and amalgam sodium (3.58 g, 7.47 mmol) were added thereto under ice-cold conditions, and the resultant mixture was stirred at the same temperature for 30 minutes, and then further stirred at room temperature for 3 hours. The reaction solution was added with a saturated aqueous solution of sodium hydrogen carbonate and extracted with diethyl ether. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and concentrated in vacuo. The obtained residue was purified by distillation, and 5-cyclopropoxy-2-methylpyridine (240 mg, yield 86%) was obtained as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08153634B2 |
| 出典データセット | uspto-grants-2012_04 |
| ORD ID | ord-f3d2aeb508bf473f89d6f27ec3af9a60 |
| 出典メモ | uspto-grants-2012_04 |