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

HRID 1979323
ノート
印刷プレビュー

反応式

HRID 1979323 の反応式
[C:1]([C:5]([CH2:7][N:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[N:12]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH2:11][CH:10]([NH:25][C:26]([NH:28][C:29]2[CH:34]=[CH:33][CH:32]=[C:31]([C:35]([O:37]CC3C=CC=CC=3)=[O:36])[CH:30]=2)=[O:27])[C:9]1=[O:45])=[O:6])([CH3:4])([CH3:3])[CH3:2]>[C].[Pd].CO>[C:1]([C:5]([CH2:7][N:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[N:12]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH2:11][CH:10]([NH:25][C:26](=[O:27])[NH:28][C:29]2[CH:30]=[C:31]([CH:32]=[CH:33][CH:34]=2)[C:35]([OH:37])=[O:36])[C:9]1=[O:45])=[O:6])([CH3:4])([CH3:2])[CH3:3]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 212019451-(1-tert-butylcarbonylmethyl-2-oxo-5-phenyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl)-3-(3-benzyloxycarbonylphenyl)urea

生成物 1

HCID 227094293-[3-(1-tert-butylcarbonylmethyl-2-oxo-5-phenyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl)ureido]benzoic acid収率 26.6%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

Methanol (20 ml) and 10% palladium carbon (68 mg) were added to 1-(1-tert-butylcarbonylmethyl-2-oxo-5-phenyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl)-3-(3-benzyloxycarbonylphenyl)urea (635 mg), the mixture was stirred at 50° C. under hydrogen atmosphere for 2 hours. The reaction mixture was filtrated, the filtrate was concentrated under reduced pressure. The residue was dissolved in 2 N aqueous sodium hydroxide, washed with ether, adjusted to pH 2 with concentrated hydrochloric acid, and extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate. The solvent was evaporated under the pressure, the mixed solvent of isopropyl ether and ethyl acetate was added to the residue for trituration, and collected by filtration, to thereby obtain 144 mg of the title compound as a colorless solid.

後処理

  1. filtrationThe reaction mixture was filtrated
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. dissolutionThe residue was dissolved in 2 N aqueous sodium hydroxide
  4. washwashed with ether
  5. extractionextracted with chloroform
  6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  7. customThe solvent was evaporated under the pressure
  8. additionthe mixed solvent of isopropyl ether and ethyl acetate was added to the residue for trituration
  9. filtrationcollected by filtration

出典と根拠

ORDレコード
ord-0b3fab76ae5c4f998aee75f779509ca8
出典データセット
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06239131B1

反応ノート

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