Potassium Carbonate → HCID 68868070, 화합물

HRID 1985222노트

반응식

HRID 1985222 반응식
[CH3:1][C:2]1[CH:30]=[CH:29][C:5]([CH2:6][N:7]2[CH:11]=[C:10]([CH2:12][CH2:13][O:14]S(C3C=CC(C)=CC=3)(=O)=O)[N:9]([CH2:25][CH2:26][CH3:27])[C:8]2=[O:28])=[CH:4][CH:3]=1.[CH2:31]([O:33][C:34](=[O:47])[C:35]([O:45][CH3:46])([CH3:44])[CH2:36][C:37]1[CH:42]=[CH:41][C:40](O)=[CH:39][CH:38]=1)[CH3:32].C([O-])([O-])=O.[K+].[K+]>CCO.O>[CH2:31]([O:33][C:34](=[O:47])[C:35]([O:45][CH3:46])([CH3:44])[CH2:36][C:37]1[CH:42]=[CH:41][C:40]([O:14][CH2:13][CH2:12][C:10]2[N:9]([CH2:25][CH2:26][CH3:27])[C:8](=[O:28])[N:7]([CH2:6][C:5]3[CH:4]=[CH:3][C:2]([CH3:1])=[CH:30][CH:29]=3)[CH:11]=2)=[CH:39][CH:38]=1)[CH3:32]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 57719269toluene-4-sulfonic acid 2-[1-(4-methyl-benzyl)-2-oxo-3-propyl-2,3-dihydro-1H-imidazol-4-yl]-ethyl esterHCID 688661503-(4-Hydroxy-phenyl)-2-methoxy-2-methyl-propionic acid ethyl ester

생성물 1

HCID 68868070HCID 68868070, 화합물수율 44%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
75 °C

실험 절차

A mixture of toluene-4-sulfonic acid 2-[1-(4-methyl-benzyl)-2-oxo-3-propyl-2,3-dihydro-1H-imidazol-4-yl]-ethyl ester (0.079 g, 0.184 mmol), 3-(4-hydroxy-phenyl)-2-methoxy-2-methyl-propionic acid ethyl ester (0.038 g, 0.169 mmol) and K2CO3 (0.047 g, 0.340 mmol) in EtOH (8 mL) was heated at 75° C. under N2 for 16 h. The reaction mixture was cooled to room temperature and quenched with aqueous 1 N HCl (1 mL). The solvent was removed in vacuo to give a residue that was diluted with water and extracted with EtOAc. The organic layer was dried (MgSO4) and the solvent removed in vacuo to afford crude product that was purified by flash chromatography using a 2:1 hexanes:acetone to afford 0.036 g (44%) 2-methoxy-2-methyl-3-(4-{2-[1-(4-methyl-benzyl)-2-oxo-3-propyl-2,3-dihydro-1H-imidazol-4-yl]-ethoxy}-phenyl)-propionic acid ethyl ester.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customquenched with aqueous 1 N HCl (1 mL)
  3. customThe solvent was removed in vacuo
  4. customto give a residue that
  5. extractionextracted with EtOAc
  6. dry with materialThe organic layer was dried (MgSO4)
  7. customthe solvent removed in vacuo
  8. customto afford crude product that
  9. customwas purified by flash chromatography

출처 및 근거

ORD 기록
ord-ad8d941e134b4950af03d7d844a4d03f
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07544812B2

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