Water → Methyl 2-amino-5-bromonicotinate

HRID 646724

反応式

HRID 646724 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 2763453Methyl 2-amino-5-bromonicotinate収率 73.9%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-43ab49ea88d541d0b6298495788b4593
出典データセット
uspto-grants-2010_04
特許番号
US07704995B2

関連ノート

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