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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
ノート
印刷プレビュー

反応式

HRID 1153752 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒HCID 218864351,4-Dioxane--water (1/1)溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f5c7b7b1ec0c4d1bb7260ba5004bd7b9
出典データセット
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04486433

反応ノート

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