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 1979475노트

반응식

HRID 1979475 반응식
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

참가 물질

4

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-0d1fb44c144d4fbdbe8b88f0770484d9
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06239131B1

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