Tetrahydrofuran → 1-(N,N-dibutylaminocarbonyloxy)-2-phenylphenanthroimidazole

HRID 622330

反応式

HRID 622330 の反応式
[OH:1][N:2]1[C:6]2[CH:7]=[CH:8][C:9]3[C:10]4[CH:11]=[CH:12][CH:13]=[CH:14][C:15]=4[CH:16]=[CH:17][C:18]=3[C:5]=2[N:4]=[C:3]1[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:31]([N:35]([CH2:39][CH2:40][CH2:41][CH3:42])[C:36](Cl)=[O:37])[CH2:32][CH2:33][CH3:34].O1CCCC1>C(OCC)(=O)C.O>[CH2:31]([N:35]([C:36]([O:1][N:2]1[C:6]2[CH:7]=[CH:8][C:9]3[C:10]4[CH:11]=[CH:12][CH:13]=[CH:14][C:15]=4[CH:16]=[CH:17][C:18]=3[C:5]=2[N:4]=[C:3]1[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[O:37])[CH2:39][CH2:40][CH2:41][CH3:42])[CH2:32][CH2:33][CH3:34]

参加物

7

反応物 4

HCID 8028TetrahydrofuranHCID 11430Potassium CarbonateHCID 83371Dibutylcarbamoyl chlorideHCID 867424231-Hydroxy-2-phenylphenanthroimidazole

生成物 1

HCID 867424221-(N,N-dibutylaminocarbonyloxy)-2-phenylphenanthroimidazole

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

10 parts of 1-hydroxy-2-phenylphenanthroimidazole, 8 parts of anhydrous potassium carbonate and 6.7 parts of N,N-dibutylcarbamyl chloride in 100 parts of tetrahydrofuran are refluxed for 5 hours. 100 parts of water and 200 parts of ethyl acetate are then added. The organic phase is washed with water, dried over sodium sulfate and evaporated down under reduced pressure. When the residue is left to stand, 6.6 parts of a solid which has a melting point of 120° C. and is pure according to thin layer chromatography are obtained.

後処理

  1. washThe organic phase is washed with water
  2. dry with materialdried over sodium sulfate
  3. customevaporated down under reduced pressure
  4. waitWhen the residue is left
  5. customare obtained

出典と根拠

ORDレコード
ord-c08a6d890a5b4754bc072ba3271cb4fa
出典データセット
uspto-grants-1988_09
特許番号
US04770976

関連ノート

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