3,5-Dimethylisoxazole-4-isocyanate → HCID 25255370、化合物

HRID 507403

反応式

HRID 507403 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:26])[CH2:9][N:10]2[C:14](=[O:15])[C:13]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)([CH2:16][CH2:17][CH3:18])[N:12]=[C:11]2[CH3:25])=[CH:4][CH:3]=1.[N:27]([C:30]1[C:31]([CH3:36])=[N:32][O:33][C:34]=1[CH3:35])=[C:28]=[O:29]>ClCCl>[CH3:36][C:31]1[C:30]([NH:27][C:28]([NH:1][C:2]2[CH:3]=[CH:4][C:5]([C:8](=[O:26])[CH2:9][N:10]3[C:14](=[O:15])[C:13]([C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)([CH2:16][CH2:17][CH3:18])[N:12]=[C:11]3[CH3:25])=[CH:6][CH:7]=2)=[O:29])=[C:34]([CH3:35])[O:33][N:32]=1

参加物

4

反応物 2

HCID 27362663,5-Dimethylisoxazole-4-isocyanateHCID 68467135HCID 68467135、化合物

生成物 1

HCID 25255370HCID 25255370、化合物収率 35.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of (+/−)-3-[2-(4-amino-phenyl)-2-oxo-ethyl]-2-methyl-5-phenyl-5-propyl-3,5-dihydro-imidazol-4-one (88 mg, 0.25 mmol) and 4-isocyanato-3,5-dimethyl-isoxazole (35 mg, 0.25 mmol) in 3 mL dichloromethane is stirred at room temperature for 18 hours. Subsequently the solvent is evaporated and the residue is dissolved in acetonitrile, the solution filtrated and subjected to preparative HPLC purification (method 3) to yield (+/−)-1-(3,5-dimethyl-isoxazol-4-yl)-3-{4-[2-(2-methyl-5-oxo-4-phenyl-4-propyl-4,5-dihydro-imidazol-1-yl)-acetyl]-phenyl}-urea (43 mg, 35%), LC/MS at 254 nm; [M+H] 488; Rt 2.648 min.

後処理

  1. customSubsequently the solvent is evaporated
  2. dissolutionthe residue is dissolved in acetonitrile
  3. filtrationthe solution filtrated
  4. customsubjected to preparative HPLC purification (method 3)

出典と根拠

ORDレコード
ord-788ec14dbf054e259be1b6dbb050e94f
出典データセット
uspto-grants-2010_08
特許番号
US07786155B2

関連ノート

読み込み中…