Hydrochloric Acid → 5-Methyl-6-(2-methylpiperidin-1-yl)nicotinic acid

HRID 1950835ノート

反応式

HRID 1950835 の反応式
[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

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14797Potassium HydroxideHCID 674005855-Methyl-6-(2-methylpiperidin-1-yl)nicotinonitrile

生成物 1

HCID 584433645-Methyl-6-(2-methylpiperidin-1-yl)nicotinic acid収率 100%

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

  1. temperatureat reflux for 16 hours
  2. extractionthe aqueous layer extracted with ethyl acetate
  3. dry with materialThe combined organic phase was dried over magnesium sulphate
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-3a9eaebbbfcb446ea01d05522044eea2
出典データセット
uspto-grants-2013_03
特許番号
US08404676B2

反応ノート

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