Sodium hydride → 2-(4-Bromo-pyrazolo[3,4-c]pyridin-1-yl)-ethanol
反応式
[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6](Br)[C:7]=1/[CH:8]=[N:9]/[NH:10][CH2:11][CH2:12][OH:13].[H-].[Na+]>C1COCC1>[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]2[N:10]([CH2:11][CH2:12][OH:13])[N:9]=[CH:8][C:7]=12参加物
4
実験手順
In analogy to GP2, 520 mg of 2-{N′-[1-(3,5-Dibromo-pyridin-4-yl)-meth-(E)-ylidene]-hydrazino}-ethanol (Intermediate 1.2, 1.61 mmol, 1 eq) were dissolved in 14 mL dry THF, treated at rt with 155 mg 50-60% sodium hydride (3.54 mmol, 2.2 eq) and subsequently refluxed for 90 min. The reaction mixture was quenched with water, extracted with ethyl acetate, the combined organic layers dried and concentrated in vacuo to yield 424 mg of a crude product, which was optionally further purified by trituration or flash column chromatography.
後処理
- temperaturesubsequently refluxed for 90 min
- customThe reaction mixture was quenched with water
- extractionextracted with ethyl acetate
- customthe combined organic layers dried
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-2adca0a3a5cb4710ac7e26ffa6d7722d
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08481539B2
反応ノート
読み込み中…