3-(2-methoxyiminopropyl)-4-(4-methoxyphenyl)-1,5,6,7-tetrahydro-2H-azepinone → HCID 20332954, 화합물

HRID 26431노트

반응식

HRID 26431 반응식
CO[N:3]=[C:4]([CH3:22])[CH2:5][C:6]1[C:7](=[O:21])[NH:8][CH2:9][CH2:10][CH2:11][C:12]=1[C:13]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][CH:14]=1.[H][H]>C(O)C.[Ni]>[NH2:3][CH:4]([CH3:22])[CH2:5][C:6]1[C:7](=[O:21])[NH:8][CH2:9][CH2:10][CH2:11][C:12]=1[C:13]1[CH:14]=[CH:15][C:16]([O:19][CH3:20])=[CH:17][CH:18]=1

참가 물질

5

반응물 2

HCID 867364713-(2-methoxyiminopropyl)-4-(4-methoxyphenyl)-1,5,6,7-tetrahydro-2H-azepinoneHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 20332954HCID 20332954, 화합물

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

The solution of 6.5 g of 3-(2-methoxyiminopropyl)-4-(4-methoxyphenyl)-1,5,6,7-tetrahydro-2H-azepinone in 150 ml of ethanol is hydrogenated at room temperature and atmospheric pressure in the presence of 10 g of Raney nickel until the uptake of 2 mole equivalents of hydrogen is complete. The mixture is filtered, the filtrate evaporated and the residue dissolved in 100 ml of water and 10 ml of 6 N hydrochloric acid. The acidic solution is washed with diethyl ether, filtered, basified with 30 ml of 3 N aqueous sodium hydroxide and repeatedly extracted with chloroform. The extract is dried, evaporated and the residue is purified by suspension in diethyl ether, to give the 3-(2-aminopropyl)-4-(4-methoxyphenyl)-1,5,6,7-tetrahydro-2H-azepinone melting at 131°-133°.

후처리

  1. customis hydrogenated at room temperature
  2. filtrationThe mixture is filtered
  3. customthe filtrate evaporated
  4. dissolutionthe residue dissolved in 100 ml of water
  5. washThe acidic solution is washed with diethyl ether
  6. filtrationfiltered
  7. extractionrepeatedly extracted with chloroform
  8. customThe extract is dried
  9. customevaporated
  10. customthe residue is purified by suspension in diethyl ether

출처 및 근거

ORD 기록
ord-b22b5f316c484a7f9559a49fc4cf3e77
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04150129

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