Potassium Carbonate → 5-Chloropyrazinoic acid

HRID 388384

反応式

HRID 388384 の反応式
[Cl:1][C:2]1[N:3]=[CH:4][C:5]([C:8]([O:10]C)=[O:9])=[N:6][CH:7]=1.C(=O)([O-])[O-].[K+].[K+]>CO.O>[Cl:1][C:2]1[N:3]=[CH:4][C:5]([C:8]([OH:10])=[O:9])=[N:6][CH:7]=1

参加物

5

反応物 2

HCID 11430Potassium CarbonateHCID 406081Methyl 5-chloropyrazine-2-carboxylate

生成物 1

HCID 4654725-Chloropyrazinoic acid収率 72.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

A solution of methyl 5-chloro-2-pyrazinecarboxylate (Bio-Farma; 1.50 g, 8.69 mmol) in a mixture of methanol (16 ml) and water (8 ml) was stirred at room temperature and treated with potassium carbonate (1.201 g, 8.69 mmol). The resulting solution was stirred for 2 hrs and the methanol removed under reduced pressure. The residue was partitioned between ethyl acetate and water (20 ml) and the aqueous layer acidified by addition of 5M hydrochloric acid. Extraction (×2) with ethyl acetate and drying over MgSO4 followed by removal of the solvent under reduced pressure, gave the title compound (1.00 g) as a white solid;

後処理

  1. stirringThe resulting solution was stirred for 2 hrs
  2. customthe methanol removed under reduced pressure
  3. customThe residue was partitioned between ethyl acetate and water (20 ml)
  4. additionthe aqueous layer acidified by addition of 5M hydrochloric acid
  5. extractionExtraction (×2) with ethyl acetate
  6. dry with materialdrying over MgSO4
  7. customfollowed by removal of the solvent under reduced pressure

出典と根拠

ORDレコード
ord-ba30737b57bc4b459ce1bb5842ea681e
出典データセット
uspto-grants-2013_02
特許番号
US08377941B2

関連ノート

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