Nitrogen → HCID 68867376, 화합물

HRID 1985220노트

반응식

HRID 1985220 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:46])[C:35]([O:38][C:39]1[CH:44]=[CH:43][C:42](O)=[CH:41][CH:40]=1)([CH3:37])[CH3:36])[CH3:32].N#N>CN(C=O)C>[CH2:31]([O:33][C:34](=[O:46])[C:35]([CH3:37])([O:38][C:39]1[CH:44]=[CH:43][C:42]([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:41][CH:40]=1)[CH3:36])[CH3:32]

참가 물질

5

반응물 3

HCID 947NitrogenHCID 181741Ethyl 2-(4-hydroxyphenoxy)-2-methylpropanoateHCID 57719269toluene-4-sulfonic acid 2-[1-(4-methyl-benzyl)-2-oxo-3-propyl-2,3-dihydro-1H-imidazol-4-yl]-ethyl ester

생성물 1

HCID 68867376HCID 68867376, 화합물수율 19.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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 (0.194 g, 1.51 mmol), 2-(4-hydroxy-phenoxy)-2-methyl-propionic acid ethyl ester (0.088 g, 0.392 mmol) and CS2CO3 (0.156 g, 0.478 mmol) in DMF (15 mL) was heated at 55° C. for under N2 for 16 h. The reaction mixture was cooled to room temperature, quenched with aqueous 1 N HCl (2 mL), and worked up extractively with EtOAc and water. The organic layer was dried (MgSO4) and the solvent removed in vacuo to afford crude product that was purified by flash chromatography using a gradient of 4:1 to 1:1 hexanes:acetone to afford 0.036 g (19%) 2-methyl-2-(4-{2-[1-(4-methyl-benzyl)-2-oxo-3-propyl-2,3-dihydro-1H-imidazol-4-yl]-ethoxy}-phenoxy)-propionic acid ethyl ester.

후처리

  1. customquenched with aqueous 1 N HCl (2 mL)
  2. dry with materialThe organic layer was dried (MgSO4)
  3. customthe solvent removed in vacuo
  4. customto afford crude product that
  5. customwas purified by flash chromatography

출처 및 근거

ORD 기록
ord-58b0f8cdf85949cebbf68281547aa1b9
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07544812B2

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