Citric Acid → HCID 70981544, 화합물

HRID 2280748노트

반응식

HRID 2280748 반응식
[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]

참가 물질

5

반응물 3

HCID 311Citric AcidHCID 14798Sodium HydroxideHCID 295702HCID 295702, 화합물

생성물 1

HCID 70981544HCID 70981544, 화합물수율 99%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-106517181ed24892bb4416d67500277b
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09139534B2

반응 노트

불러오는 중…