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Sodium Hydroxide → 2-Amino-7-(p-chloro-benzoyl)-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine

HRID 1153752
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HRID 1153752 반응식
[Cl:1][C:2]1[CH:18]=[CH:17][C:5]([C:6]([N:8]2[CH2:14][CH2:13][C:12](=O)[C:11](=O)[CH2:10][CH2:9]2)=[O:7])=[CH:4][CH:3]=1.ClC1C=CC(C(N2CCCC(=O)CC2)=O)=CC=1.[Se](=O)=O.Br.Br.[NH2:41][CH2:42][C:43]([NH2:45])=[NH:44].[OH-].[Na+]>O1CCOCC1.O.CO.C(OCC)(=O)C>[NH2:45][C:43]1[CH:42]=[N:41][C:12]2[CH2:13][CH2:14][N:8]([C:6](=[O:7])[C:5]3[CH:17]=[CH:18][C:2]([Cl:1])=[CH:3][CH:4]=3)[CH2:9][CH2:10][C:11]=2[N:44]=1
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참가 물질

9

반응물 5

HCID 14798Sodium HydroxideHCID 24007Selenium DioxideHCID 16211382Aminoacetamidine DihydrobromideHCID 204364131-(4-Chloro-benzoyl)-hexahydroazepine-4-oneHCID 204364431-(4-Chloro-benzoyl)-hexahydroazepine-4,5-dione

생성물 1

HCID 130370422-Amino-7-(p-chloro-benzoyl)-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine

시약·촉매·용매 3

HCID 887Methanol용매HCID 8857Ethyl Acetate용매HCID 218864351,4-Dioxane--water (1/1)용매

실험 절차

53 mg (0.2 mol) of a mixture of 1-(4-chloro-benzoyl)-hexahydroazepine-4,5-dione and 1-(4-chloro-benzoyl)-hexhydroazepine-3,4-dione [prepared from 1-(4-chloro-benzoyl)-hexahydroazepine-4-one by selenium dioxide oxidation in dioxane/water] and 47 gm (0.2 mol) of 2-amino-acetamidine dihydrobromide were dissolved in 700 ml of methanol, and 200 ml of 2N sodium hydroxide were added dropwise to the solution at 5° C. The mixture was stirred at room temperature for one hour, then concentrated by evaporation and then, after addition of more sodium hydroxide, extracted with chloroform. The dried extract solution was concentrated by evaporation and chromatographed on silicagel with ethyl acetate/methanol (10:1) as the mobile phase. The crystals obtained thereby were digested with ethyl acetate and suction-filtered.

후처리

  1. concentrationconcentrated by evaporation
  2. additionafter addition of more sodium hydroxide
  3. extractionextracted with chloroform
  4. extractionThe dried extract solution
  5. concentrationwas concentrated by evaporation
  6. customchromatographed on silicagel with ethyl acetate/methanol (10:1) as the mobile phase
  7. customThe crystals obtained
  8. filtrationsuction-filtered

출처 및 근거

ORD 기록
ord-f5c7b7b1ec0c4d1bb7260ba5004bd7b9
출처 데이터셋
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04486433

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