Lithium Hydroxide → 3-Nitropyridine-2-carboxylic acid

HRID 2300930

반응식

HRID 2300930 반응식
C([O:3][C:4]([C:6]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[CH:8][N:7]=1)=[O:5])C.[OH-].[Li+]>CO.O>[C:4]([C:6]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[CH:8][N:7]=1)([OH:5])=[O:3]

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 18376573Ethyl 3-nitropyridine-2-carboxylate

생성물 1

HCID 183766123-Nitropyridine-2-carboxylic acid수율 95%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

To a solution of 2-ethoxycarbonyl-3-nitropyridine (0.5 g, 2.5 mmoL, 1 eq.) in 20 mL of methanol and 5 mL of water was added lithium hydroxide (0.2 g, 4.5 mmoL, 1.8 eq.) and the mixture stirred for 16 hours at ambient temperature. The reaction was concentrated and 50 mL of 1N KOH was were added. The solution was washed with 25 mL of ethyl actetate, acidified with 1 N HCl, and extracted with ethyl acetate (3×50 mL). The combined ethyl acetate extractions were dried over sodium sulfate and concentrated to give 2-carboxy-3-nitropyridine as a yellow solid (0.4 g, 95% yield).

후처리

  1. concentrationThe reaction was concentrated
  2. addition50 mL of 1N KOH was were added
  3. washThe solution was washed with 25 mL of ethyl actetate
  4. extractionextracted with ethyl acetate (3×50 mL)
  5. extractionThe combined ethyl acetate extractions
  6. dry with materialwere dried over sodium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-5c74b095b3ed481fbd2380c6aa8b9e24
출처 데이터셋
uspto-grants-2002_12
특허 번호
US06498185B1

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