Water → HCID 178457923、化合物

HRID 1930740ノート

反応式

HRID 1930740 の反応式
[O:1]([CH2:8][C:9]1[NH:10][CH:11]=[C:12]([C:14]2[CH:27]=[CH:26][C:17]([O:18][C:19]3[CH:25]=[CH:24][C:22]([NH2:23])=[CH:21][CH:20]=3)=[CH:16][CH:15]=2)[N:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:28]([N:31]=[C:32]=[O:33])([CH3:30])[CH3:29].O.C(OCC)(=O)C>CN(C)C=O>[CH:28]([NH:31][C:32]([NH:23][C:22]1[CH:21]=[CH:20][C:19]([O:18][C:17]2[CH:26]=[CH:27][C:14]([C:12]3[N:13]=[C:9]([CH2:8][O:1][C:2]4[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=4)[NH:10][CH:11]=3)=[CH:15][CH:16]=2)=[CH:25][CH:24]=1)=[O:33])([CH3:30])[CH3:29]

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 61277Isopropyl isocyanateHCID 178507748HCID 178507748、化合物

生成物 1

HCID 178457923HCID 178457923、化合物収率 20%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

A mixture containing 4-{4-[2-(phenoxymethyl)-1H-imidazol-4-yl]phenoxy}aniline (0.2 g, 0.56 mmol) and isopropylisocyanate (0.155 g, 1.8 mmol) in 3 ml of dimethylformamide is heated at 100° C. for two hours then stirred at ambient temperature for two hours. 20 ml of water and 30 ml of ethyl acetate are added, followed by extraction, then the organic phase is washed with a saturated sodium chloride solution. The organic phase is dried over sodium sulfate. After evaporation to dryness, the oil obtained is triturated in isopentane. After filtration then drying, the solid obtained is purified on a silica column (eluent dichloromethane-ethanol-ammonia 96/2/2) and a pink-cream coloured powder is obtained with a yield of 20%.

後処理

  1. extractionfollowed by extraction
  2. washthe organic phase is washed with a saturated sodium chloride solution
  3. dry with materialThe organic phase is dried over sodium sulfate
  4. customAfter evaporation to dryness
  5. customthe oil obtained
  6. customis triturated in isopentane
  7. filtrationAfter filtration
  8. customthen drying
  9. customthe solid obtained
  10. customis purified on a silica column (eluent dichloromethane-ethanol-ammonia 96/2/2)
  11. customis obtained with a yield of 20%

出典と根拠

ORDレコード
ord-82406d6e907e43dfa1a27ad477627afd
出典データセット
uspto-grants-2012_05
特許番号
US08188133B2

反応ノート

読み込み中…