Lithium Hydroxide → 2-aminopyrimidine-5-carboxylic Acid

HRID 1259486ノート

反応式

HRID 1259486 の反応式
[NH2:1][C:2]1[N:7]=[CH:6][C:5]([C:8]([O:10]C)=[O:9])=[CH:4][N:3]=1.[OH-].[Li+]>CO.O>[NH2:1][C:2]1[N:7]=[CH:6][C:5]([C:8]([OH:10])=[O:9])=[CH:4][N:3]=1

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 9793866Methyl 2-aminopyrimidine-5-carboxylate

生成物 1

HCID 70203672-aminopyrimidine-5-carboxylic Acid

試薬・触媒・溶媒 2

HCID 962Water触媒HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

Methyl 2-aminopyrimidine-5-carboxylate (300 mg, 2.0 mmol) was diluted in methanol (5 mL) containing a few drops of water. Lithium hydroxide (122 mg, 5.1 mmol) was added, and the reaction mixture was stirred at 60° C. overnight. The mixture was concentrated under reduced pressure, then diluted in water and adjusted to pH 4 with 1 M HCl. 2-Aminopyrimidine-5-carboxylic acid precipitated as a white solid, which was isolated by vacuum filtration (244 mg, 90%): 1H NMR (DMSO-d6) δ: 12.73 (1H, br s), 8.63 (2H, s), 7.44 (2H, br s).

後処理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. additiondiluted in water
  3. custom2-Aminopyrimidine-5-carboxylic acid precipitated as a white solid
  4. customwhich was isolated by vacuum filtration (244 mg, 90%)

出典と根拠

ORDレコード
ord-bdc6f0c42e774fc7bff59ebd795fa7a1
出典データセット
uspto-grants-2013_06
特許番号
US08466283B2

反応ノート

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