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

HRID 26431ノート

反応式

HRID 26431 の反応式
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

参加物

5

反応物 2

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

生成物 1

HCID 20332954HCID 20332954、化合物

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-b22b5f316c484a7f9559a49fc4cf3e77
出典データセット
uspto-grants-1979_04
特許番号
US04150129

反応ノート

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