Phenyl isocyanate → 1-(1-tert-butylcarbonylmethyl-2-oxo-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl)-3-phenylurea

HRID 1979469노트

반응식

HRID 1979469 반응식
[C:1]1([N:7]=[C:8]=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:10]([C:14]([CH2:16][N:17]1[C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=2[N:21]([CH:28]2[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]2)[CH2:20][CH:19]([NH2:34])[C:18]1=[O:35])=[O:15])([CH3:13])([CH3:12])[CH3:11]>O1CCCC1>[C:10]([C:14]([CH2:16][N:17]1[C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=2[N:21]([CH:28]2[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]2)[CH2:20][CH:19]([NH:34][C:8]([NH:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[O:9])[C:18]1=[O:35])=[O:15])([CH3:13])([CH3:11])[CH3:12]

참가 물질

4

반응물 2

HCID 7672Phenyl isocyanateHCID 154908351-tert-butylcarbonylmethyl-2-oxo-3-amino-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine

생성물 1

HCID 212015561-(1-tert-butylcarbonylmethyl-2-oxo-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl)-3-phenylurea수율 84%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Phenyl isocyanate (110 mg) was added to a solution of 1-tert-butylcarbonylmethyl-2-oxo-3-amino-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (300 mg) in anhydrous tetrahydrofuran (10 ml), the mixture was stirred for 10 minutes at room temperature. The reaction mixture was concentrated under reduced pressure, etanol was added to the residue for crystallization, collected by filtration, to thereby obtain 336 mg of the title compound (Yield 83.9%).

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-18dd72bdc1914fd8a73714011bb28c5e
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06239131B1

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