Potassium Carbonate → 5-Chloropyrazinoic acid

HRID 388384

반응식

HRID 388384 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 4654725-Chloropyrazinoic acid수율 72.6%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

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;

후처리

  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

출처 및 근거

ORD 기록
ord-ba30737b57bc4b459ce1bb5842ea681e
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08377941B2

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