Water → Methyl 2-amino-5-bromonicotinate

HRID 646724

반응식

HRID 646724 반응식
[NH2:1][C:2]1[C:7]([C:8]([OH:10])=[O:9])=[CH:6][C:5]([Br:11])=[CH:4][N:3]=1.OS(O)(=O)=O.O.[C:18](=O)([O-])[O-].[Na+].[Na+]>CO.C(OCC)(=O)C>[NH2:1][C:2]1[C:7]([C:8]([O:10][CH3:18])=[O:9])=[CH:6][C:5]([Br:11])=[CH:4][N:3]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 7374452-Amino-5-bromonicotinic acid

생성물 1

HCID 2763453Methyl 2-amino-5-bromonicotinate수율 73.9%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

A slurry of 2-amino-5-bromopyridine-3-carboxylic acid (7 g, 32.2 mmol) in methanol (150 mL) and H2SO4 (7 mmol) was heated to reflux for 48 h. The reaction mixture was concentrated to ca. 40 mL. Water (100 mmol) was added to the residual oil, and the mixture neutralized with sodium carbonate. Ethyl acetate (400 mL) was added and the organic layer was washed with saturated aqueous sodium chloride then dried (Na2SO4) and concentrated to give the title compound (5.5 g, 73.9% yield).

후처리

  1. temperatureto reflux for 48 h
  2. concentrationThe reaction mixture was concentrated to ca. 40 mL
  3. washthe organic layer was washed with saturated aqueous sodium chloride
  4. dry with materialthen dried (Na2SO4)
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-43ab49ea88d541d0b6298495788b4593
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07704995B2

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