Lithium Hydroxide → 3-Nitropyridine-2-carboxylic acid

HRID 370101

反応式

HRID 370101 の反応式
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]

参加物

5

反応物 2

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

生成物 1

HCID 183766123-Nitropyridine-2-carboxylic acid収率 95%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-bc6e07d8479841b9a26da54b98fc628b
出典データセット
uspto-grants-2000_10
特許番号
US06140351

関連ノート

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