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Hydrochloric Acid → 3-(2-piperidinopropyl)-4-(3-methoxyphenyl)-1,5,6,7-tetrahydro-2H-azepinone

HRID 26419
ノート
印刷プレビュー

反応式

HRID 26419 の反応式
[CH2:1]([C:5]1[C:6](=[O:20])[NH:7][CH2:8][CH2:9][CH2:10][C:11]=1[C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([O:18][CH3:19])[CH:13]=1)[C:2]([CH3:4])=O.[NH:21]1[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1.Cl.C([BH3-])#N.[Na+]>CO>[N:21]1([CH:2]([CH3:4])[CH2:1][C:5]2[C:6](=[O:20])[NH:7][CH2:8][CH2:9][CH2:10][C:11]=2[C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([O:18][CH3:19])[CH:13]=2)[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric Acid2 回HCID 8082PiperidineHCID 5003444Sodium cyanoborohydride2 回HCID 203329343-acetonyl-4-(3-methoxyphenyl)-1,5,6,7-tetrahydro-2H-azepinone

生成物 1

HCID 203329443-(2-piperidinopropyl)-4-(3-methoxyphenyl)-1,5,6,7-tetrahydro-2H-azepinone

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

実験手順

The solution of 8.0 g of 3-acetonyl-4-(3-methoxyphenyl)-1,5,6,7-tetrahydro-2H-azepinone, 14.95 g of piperidine, 6.6 ml of 5 N methanolic hydrogen chloride and 1.9 g of sodium cyanoborohydride in 120 ml of methanol is refluxed overnight. An additional portion of 0.95 g of sodium cyanoborohydride is added and refluxing continued for 24 hours. The mixture is cooled to 0°, 30 ml of concentrated hydrochloric acid are added and the solution concentrated. The concentrate is diluted with 100 ml of water, the solution washed with benzene and rendered basic with 70 ml of 3 N aqueous sodium hydroxide. It is extracted with diethyl ether, the extract evaporated and the residue crystallized from petroleum ether and hexane, to yield the 3-(2-piperidinopropyl)-4-(3-methoxyphenyl)-1,5,6,7-tetrahydro-2H-azepinone of the formula ##STR7## melting at 97° to 99°.

後処理

  1. temperaturerefluxing
  2. temperatureThe mixture is cooled to 0°
  3. concentrationthe solution concentrated
  4. additionThe concentrate is diluted with 100 ml of water
  5. washthe solution washed with benzene
  6. extractionIt is extracted with diethyl ether
  7. customthe extract evaporated
  8. customthe residue crystallized from petroleum ether and hexane

出典と根拠

ORDレコード
ord-481dd5b797924028a82d5f5e0d0d8591
出典データセット
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04150129

反応ノート

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