Citric Acid → HCID 70981544、化合物

HRID 2280748ノート

反応式

HRID 2280748 の反応式
[C:1]([NH:5][C:6]1[C:11]([C:12]([O:14]CC)=[O:13])=[CH:10][N:9]=[C:8]([S:17][CH3:18])[N:7]=1)([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>C(O)C>[C:1]([NH:5][C:6]1[C:11]([C:12]([OH:14])=[O:13])=[CH:10][N:9]=[C:8]([S:17][CH3:18])[N:7]=1)([CH3:4])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 311Citric AcidHCID 14798Sodium HydroxideHCID 295702HCID 295702、化合物

生成物 1

HCID 70981544HCID 70981544、化合物収率 99%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In a round-bottomed flask ethyl 4-(tert-butylamino)-2-(methylthio)pyrimidine-5-carboxylate (3.2 g, 11.88 mmol) was dissolved in ethanol (40 mL) followed by the addition of 1M aqueous sodium hydroxide solution (35.6 mL, 35.6 mmol). The resulting mixture was stirred overnight at room temperature and then the solvent was evaporated under reduced pressure. After that 2M aqueous citric acid solution (35.6 mL, 71.3 mmol) was slowly added and the resulting mixture was stirred for 0.5 h at room temperature. The suspension was filtered and the solids were washed twice with water (2×50 mL) and then dried in a vacuum oven at 45° C. overnight to afford 4-(tert-butylamino)-2-(methylthio)pyrimidine-5-carboxylic acid (2.83 g, 11.73 mmol, 99% yield). MS (ESI) m/z 242.3 [M+1]+.

後処理

  1. customthe solvent was evaporated under reduced pressure
  2. stirringthe resulting mixture was stirred for 0.5 h at room temperature
  3. filtrationThe suspension was filtered
  4. washthe solids were washed twice with water (2×50 mL)
  5. customdried in a vacuum oven at 45° C. overnight

出典と根拠

ORDレコード
ord-106517181ed24892bb4416d67500277b
出典データセット
uspto-grants-2015_09
特許番号
US09139534B2

反応ノート

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