Hydrochloric Acid → 5-Methyl-6-(2-methylpiperidin-1-yl)nicotinic acid
反応式
[CH3:1][C:2]1[C:3]([N:10]2[CH2:15][CH2:14][CH2:13][CH2:12][CH:11]2[CH3:16])=[N:4][CH:5]=[C:6]([CH:9]=1)[C:7]#N.[OH-:17].[K+].Cl.[OH2:20]>>[CH3:1][C:2]1[C:3]([N:10]2[CH2:15][CH2:14][CH2:13][CH2:12][CH:11]2[CH3:16])=[N:4][CH:5]=[C:6]([CH:9]=1)[C:7]([OH:20])=[O:17]参加物
5
実験手順
A mixture of 5-methyl-6-(2-methylpiperidin-1-yl)nicotinonitrile (1 g; 4.64 mmol; 1 eq.) and potassium hydroxide (1.3 g; 23.2 mmol; 5 eq.) in water (60 mL) was stirred at reflux for 16 hours. The pH was adjusted to 5-6 with HCl 1M and the aqueous layer extracted with ethyl acetate. The combined organic phase was dried over magnesium sulphate and concentrated in vacuo to afford the title compound (1.1 g, 100%) as a yellow oil.
後処理
- temperatureat reflux for 16 hours
- extractionthe aqueous layer extracted with ethyl acetate
- dry with materialThe combined organic phase was dried over magnesium sulphate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-b7010f80ee3f4bffa8fac792d95bcaa3
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08889668B2
反応ノート
読み込み中…