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

HRID 336261노트

반응식

HRID 336261 반응식
[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]

참가 물질

5

반응물 4

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b7010f80ee3f4bffa8fac792d95bcaa3
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08889668B2

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