Nitrogen → HCID 68867376、化合物

HRID 1985220

反応式

HRID 1985220 の反応式
[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]

参加物

5

反応物 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

生成物 1

HCID 68867376HCID 68867376、化合物収率 19.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-58b0f8cdf85949cebbf68281547aa1b9
出典データセット
uspto-grants-2009_06
特許番号
US07544812B2

関連ノート

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