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

HRID 26419
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HRID 26419 반응식
[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
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참가 물질

6

반응물 4

HCID 313Hydrochloric Acid2회HCID 8082PiperidineHCID 5003444Sodium cyanoborohydride2회HCID 203329343-acetonyl-4-(3-methoxyphenyl)-1,5,6,7-tetrahydro-2H-azepinone

생성물 1

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

시약·촉매·용매 1

HCID 887
Methanol
용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-481dd5b797924028a82d5f5e0d0d8591
출처 데이터셋
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04150129

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