Trifluoroacetic acid → 3-[3-(1-cyclohexylcarbonylmethyl-2-oxo-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl)ureido]benzoic acid

HRID 1979475ノート

反応式

HRID 1979475 の反応式
FC(F)(F)C(O)=O.[CH:8]1([C:14]([CH2:16][N:17]2[C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=3[N:21]([CH:28]3[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]3)[CH2:20][CH:19]([NH:34][C:35]([NH:37][C:38]3[CH:43]=[CH:42][CH:41]=[C:40]([C:44]([O:46]C(C)(C)C)=[O:45])[CH:39]=3)=[O:36])[C:18]2=[O:51])=[O:15])[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1>C(Cl)Cl>[CH:8]1([C:14]([CH2:16][N:17]2[C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=3[N:21]([CH:28]3[CH2:29][CH2:30][CH2:31][CH2:32][CH2:33]3)[CH2:20][CH:19]([NH:34][C:35](=[O:36])[NH:37][C:38]3[CH:39]=[C:40]([CH:41]=[CH:42][CH:43]=3)[C:44]([OH:46])=[O:45])[C:18]2=[O:51])=[O:15])[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 212018681-(1-cyclohexylcarbonylmethyl-2-oxo-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl)-3-(3-tert-butoxycarbonylphenyl)urea

生成物 1

HCID 212020303-[3-(1-cyclohexylcarbonylmethyl-2-oxo-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl)ureido]benzoic acid収率 65%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Trifluoroacetic acid (5 ml) was added to a solution of 1-(1-cyclohexylcarbonylmethyl-2-oxo-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl)-3-(3-tert-butoxycarbonylphenyl)urea (560 mg) in methylene chloride (5 ml), the mixture was stirred at room temperature for one hour. The reaction mixture was concentrated under reduced pressure, etanol was added to the residue for crystallization, collected by filtration, to thereby obtain 330 mg of the title compound.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure, etanol
  2. additionwas added to the residue for crystallization
  3. filtrationcollected by filtration

出典と根拠

ORDレコード
ord-0d1fb44c144d4fbdbe8b88f0770484d9
出典データセット
uspto-grants-2001_05
特許番号
US06239131B1

反応ノート

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