1-(1-tert-butoxycarbonylmethyl-2-oxo-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl)-3-(3-benzyloxycarbonylphenyl)urea → 3-[3-(1-tert-butoxycarbonylmethyl-2-oxo-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl)ureido]benzoic acid

HRID 1979484ノート

反応式

HRID 1979484 の反応式
[C:1]([O:5][C:6]([CH2:8][N:9]1[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=2[N:13]([CH:20]2[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]2)[CH2:12][CH:11]([NH:26][C:27]([NH:29][C:30]2[CH:35]=[CH:34][CH:33]=[C:32]([C:36]([O:38]CC3C=CC=CC=3)=[O:37])[CH:31]=2)=[O:28])[C:10]1=[O:46])=[O:7])([CH3:4])([CH3:3])[CH3:2]>C(O)C.[C].[Pd]>[C:1]([O:5][C:6]([CH2:8][N:9]1[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=2[N:13]([CH:20]2[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]2)[CH2:12][CH:11]([NH:26][C:27](=[O:28])[NH:29][C:30]2[CH:31]=[C:32]([CH:33]=[CH:34][CH:35]=2)[C:36]([OH:38])=[O:37])[C:10]1=[O:46])=[O:7])([CH3:4])([CH3:2])[CH3:3]

参加物

4

反応物 1

HCID 212017101-(1-tert-butoxycarbonylmethyl-2-oxo-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl)-3-(3-benzyloxycarbonylphenyl)urea

生成物 1

HCID 212019863-[3-(1-tert-butoxycarbonylmethyl-2-oxo-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl)ureido]benzoic acid収率 54.7%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 702Ethanol溶媒

実験手順

5% Palladium carbon (300 mg) was added to a solution of 1-(1-tert-butoxycarbonylmethyl-2-oxo-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl)-3-(3-benzyloxycarbonylphenyl)urea (960 mg) in ethanol (50 ml), the mixture was stirred at room temperature for 3 hours under hydrogen atmosphere. The reaction mixture was filtrated through a pad of Celite, and the filtrate was concentrated under reduced pressure. Isopropyl alcohol was added to the residue for crystallization, collected by filtrated, to thereby obtain 450 mg of the titled compound.

後処理

  1. filtrationThe reaction mixture was filtrated through a pad of Celite
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionIsopropyl alcohol was added to the residue for crystallization
  4. customcollected
  5. filtrationby filtrated

出典と根拠

ORDレコード
ord-339ac69fe1fd44d8bdab808f71187d1e
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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