Hydrochloric Acid → 6H-Benzo[b]quinolizin-6-one, 1,2,3,4,11,11a-hexahydro-

HRID 583255노트

반응식

HRID 583255 반응식
[CH2:1]1[C:10]2[N:5]([C:6](=[O:15])[C:7]3[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=3[CH:9]=2)[CH2:4][CH2:3][CH2:2]1.Cl>C(O)C.[Pd]>[CH2:1]1[CH:10]2[N:5]([C:6](=[O:15])[C:7]3[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=3[CH2:9]2)[CH2:4][CH2:3][CH2:2]1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 12730636HCID 12730636, 화합물

생성물 1

HCID 27527926H-Benzo[b]quinolizin-6-one, 1,2,3,4,11,11a-hexahydro-수율 94%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

To a solution of 1,3,4,6-tetrahydro-2H-benzo[b]quinolizin-6-one (4.02 g, 20.2 mmol) (M. A. Haimova, V. I. Ognyanov, and N. M. Mollov, Synthesis, 1980, 845) in ethanol (250 ml) and 2.5M hydrochloric acid (10 ml) was added 10% palladium-on-carbon (0.8 g) and the solution was shaken on a Parr Hydrogenator for 72 h. The catalyst was filtered off and the filtrate was concentrated to give an oil which was partitioned between ethyl acetate and dilute base. The dried (magnesium sulfate) organic phase was concentrated in vacuo and then placed on a high vacuum system to give the title compound as a white solid (3.8 g, 94%), m.p. 88-92° C.

후처리

  1. filtrationThe catalyst was filtered off
  2. concentrationthe filtrate was concentrated
  3. customto give an oil which
  4. customwas partitioned between ethyl acetate
  5. additiondilute base
  6. dry with materialThe dried (magnesium sulfate) organic phase
  7. concentrationwas concentrated in vacuo

출처 및 근거

ORD 기록
ord-af9282bc18b04270b5bced1947c83fce
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05929085

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