hexahydro-7-[(4-nitrophenyl)methyl]-2H-azepin-2-one → HCID 23342835, 화합물

HRID 27438노트

반응식

HRID 27438 반응식
[N+:1]([C:4]1[CH:18]=[CH:17][C:7]([CH2:8][CH:9]2[NH:15][C:14](=O)[CH2:13][CH2:12][CH2:11][CH2:10]2)=[CH:6][CH:5]=1)([O-])=O>C(O)C.[Pt].[H][H]>[NH2:1][C:4]1[CH:18]=[CH:17][C:7]([CH2:8][CH:9]2[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][NH:15]2)=[CH:6][CH:5]=1

참가 물질

4

반응물 1

HCID 11970558hexahydro-7-[(4-nitrophenyl)methyl]-2H-azepin-2-one

생성물 1

HCID 23342835HCID 23342835, 화합물

시약·촉매·용매 2

HCID 178506450HCID 178506450, 화합물촉매HCID 702Ethanol용매

실험 절차

Hydrogenate 3.72 of 7-(4-nitrobenzyl)perhydroazepin-2-one in 50 mls of ethyl alcohol with platinum/hydrogen. After the absorption of hydrogen has ceased, filter off the catalyst and concentrate the filtrate. Dissolve the thus obtained 7-(4-aminobenzyl)-perhydroazepin-2-one in tetrahydrofuran. Add 680 mg of lithium aluminum hydride and boil the mixture under reflux. After cooling, treat it with ice-water and extract it with diethyl Dry the organic phase over sodium sulphate and concentrate it to obtain 2.0 g of the brown oily title compound.

후처리

  1. customAfter the absorption of hydrogen
  2. filtrationfilter off the catalyst
  3. concentrationconcentrate the filtrate
  4. dissolutionDissolve the thus obtained 7-(4-aminobenzyl)-perhydroazepin-2-one in tetrahydrofuran
  5. additionAdd 680 mg of lithium aluminum hydride and boil the mixture
  6. temperatureunder reflux
  7. temperatureAfter cooling
  8. additiontreat it with ice-water
  9. extractionextract it with diethyl
  10. dry with materialDry the organic phase over sodium sulphate
  11. concentrationconcentrate it

출처 및 근거

ORD 기록
ord-216ecf3061c4435bb488641f80fd0567
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04221788

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