Chloroacetic Acid → 1(2H)-Pyrazineacetic acid, 2-oxo-

HRID 887113

반응식

HRID 887113 반응식
[NH:1]1[CH:6]=[CH:5][N:4]=[CH:3][C:2]1=[O:7].[OH-].[Na+].Cl[CH2:11][C:12]([OH:14])=[O:13].Cl>>[O:7]=[C:2]1[CH:3]=[N:4][CH:5]=[CH:6][N:1]1[CH2:11][C:12]([OH:14])=[O:13]

참가 물질

5

반응물 4

HCID 300Chloroacetic AcidHCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 727581,2-Dihydropyrazin-2-one

생성물 1

HCID 217140981(2H)-Pyrazineacetic acid, 2-oxo-

반응 조건

온도
100 °C

실험 절차

Pyrazin-2(1H)-one (0.333 g, 3.47 mmol) was added 5 N sodium hydroxide solution (2.1 mL) followed by chloroacetic acid (0.524 g, 5.54 mmol). The reaction mixture was heated at 100° C. for 2 h. After cooled down to ambient temperature, 2 N hydrochloric acid (3.5 mL) was added and the reaction mixture was directly purified by reverse phase HPLC (TMC Pro-Pac C18; 0-40% 0.1% trifluoroacetic acid in acetonitrile/0.1% trifluoroacetic acid in water gradient). The pure fractions were lyophilized overnight to yield the title compound as a yellow solid. LC/MS 155.2 (M+1).

후처리

  1. temperatureAfter cooled down to ambient temperature
  2. customthe reaction mixture was directly purified by reverse phase HPLC (TMC Pro-Pac C18; 0-40% 0.1% trifluoroacetic acid in acetonitrile/0.1% trifluoroacetic acid in water gradient)

출처 및 근거

ORD 기록
ord-3cd525f9d558450cb86154a3b5790845
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08247415B2

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