Ammonium Hydroxide → 2-(1-Methylcyclopropyl)pyridin-4(1H)-one
反応式
[CH3:1][C:2]1([C:5]2O[CH:7]=[CH:8][C:9](=[O:11])[CH:10]=2)[CH2:4][CH2:3]1.[OH-].[NH4+:13]>>[CH3:1][C:2]1([C:5]2[NH:13][CH:7]=[CH:8][C:9](=[O:11])[CH:10]=2)[CH2:4][CH2:3]1参加物
3
実験手順
A mixture of 2-(1-methyl-cyclopropyl)-pyran-4-one (Step 1.6) (66.6 mmol) and a 28-30% aqueous solution of ammonium hydroxide (182 mL) was stirred for 1 h at 65° C. After cooling to rt, the reaction mixture was decanted to remove a dark brown solid and then concentrated. The residue was diluted with MeOH and re-concentrated (3×) to afford the title compound as a brown-orange solid. HPLC: tR=3.56 min (method B); LC-MS: tR=0.87 min, [M+H]+ 151; TLC: Rf=0.18 (9:1 CH2Cl2/MeOH).
後処理
- customthe reaction mixture was decanted
- customto remove a dark brown solid
- concentrationconcentrated
- additionThe residue was diluted with MeOH
- concentrationre-concentrated (3×)
出典と根拠
- ORDレコード
- ord-8be7b91bf069441195fde5d3549a121e
- 出典データセット
- uspto-grants-2012_10
- 特許番号
- US08293753B2
反応ノート
読み込み中…