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Methanol → 2-Amino-5-bromo-alpha-(2-pyridyl)benzyl alcohol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | 2-Amino-5-bromophenyl-2-pyridylketone | HCID 69947412 | — |
| 生成物 | 2-Amino-5-bromo-alpha-(2-pyridyl)benzyl alcohol | HCID 12915500 | — |
反応手順
In 100 ml of methanol was dissolved 10 g of 2-amino-5-bromophenyl-2-pyridylketone. To the solution was added 1.7 g of sodium borohydride and stirred for 30 minutes. The solvent methanol was evaporated off under reduced pressure. The residue was treated with an aqueous solution of hydrochloric acid. The decomposed residue was then neutralized with 200 ml of a sodium bicarbonate aqueous solution, and extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent, hexane:ethyl acetate=2:1) to give 2-amino-5-bromo-α-(2-pyridyl)benzyl alcohol (9.0 g) as prisms, m.p. 104°-105° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05726306 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-b73af90813ea458ca97a1404afcbed16 |
| 出典メモ | uspto-grants-1998_03 |