Water → HCID 178425601、化合物

HRID 1930742ノート

反応式

HRID 1930742 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.[CH3:28][C:29]1[CH:38]=[CH:37][C:32]([CH2:33][N:34]=[C:35]=[O:36])=[CH:31][CH:30]=1.O.C(OCC)(=O)C>CN(C)C=O.C(OCC)C.C(OCC)(=O)C.C(O)(C)C>[CH3:28][C:29]1[CH:38]=[CH:37][C:32]([CH2:33][NH:34][C:35]([NH:23][C:22]2[CH:21]=[CH:20][C:19]([O:18][C:17]3[CH:26]=[CH:27][C:14]([C:12]4[N:13]=[C:9]([CH2:8][O:1][C:2]5[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=5)[NH:10][CH:11]=4)=[CH:15][CH:16]=3)=[CH:25][CH:24]=2)=[O:36])=[CH:31][CH:30]=1

参加物

7

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 27333881-(Isocyanatomethyl)-4-methylbenzeneHCID 178507748HCID 178507748、化合物

生成物 1

HCID 178425601HCID 178425601、化合物収率 21%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 86632829Ethyl ether ethyl acetate isopropanol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 4-methylbenzylisocyanate (0.17 g, 1.12 mmol) in 3 ml of dimethylformamide is heated at 100° C. for two hours. After returning to ambient temperature 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, filtered and concentrated to dryness under vacuum. The solid obtained is stirred in 5 ml of a mixture of solvents such as ethyl ether/ethyl acetate/isopropanol 6/3/1. The solid obtained is filtered then dried. A cream-coloured powder is obtained with a yield of 21%.

後処理

  1. customAfter returning to ambient temperature
  2. additionare added
  3. extractionfollowed by extraction
  4. washthe organic phase is washed with a saturated sodium chloride solution
  5. dry with materialThe organic phase is dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated to dryness under vacuum
  8. customThe solid obtained
  9. customThe solid obtained
  10. filtrationis filtered
  11. customthen dried
  12. customA cream-coloured powder is obtained with a yield of 21%

出典と根拠

ORDレコード
ord-5c0fb58a60704955a35090b46c82116f
出典データセット
uspto-grants-2012_05
特許番号
US08188133B2

反応ノート

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