HCID 21584328, 화합물 → HCID 21584267, 화합물

HRID 583258노트

반응식

HRID 583258 반응식
[ClH:1].[N+:2]([C:5]1[CH:18]=[CH:17][C:8]2[CH2:9][CH:10]3[N:15]([CH2:16][C:7]=2[CH:6]=1)[CH2:14][CH2:13][CH2:12][CH2:11]3)([O-])=O>C(O)C.[Pd]>[ClH:1].[CH2:11]1[CH:10]2[N:15]([CH2:16][C:7]3[CH:6]=[C:5]([NH2:2])[CH:18]=[CH:17][C:8]=3[CH2:9]2)[CH2:14][CH2:13][CH2:12]1

참가 물질

4

반응물 1

HCID 21584328HCID 21584328, 화합물

생성물 1

HCID 21584267HCID 21584267, 화합물수율 95.3%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

8-Nitro-1,3,4,6,11,11a-hexahydro-2H-benzo[b]quinolizine hydrochloride (2.93 g, 10.9 mmol) was dissolved in ethanol (150 ml) and 10% palladium-on-carbon (0.4 g) was added and the solution was shaken on a Parr Hydrogenator for 2 h. The catalyst was filtered off and the catalyst was washed with water. The filtrate was concentrated and absolute ethanol was added and evaporated to drive off excess water. The resulting solid was taken up in hot ethanol (75 ml) and ether (100 ml) was added slowly. The precipitate which formed was collected and dried in the air to give the title compound as an off-white solid (2.48 g, 95%), m.p. 241-3° C. (dec.).

후처리

  1. filtrationThe catalyst was filtered off
  2. washthe catalyst was washed with water
  3. concentrationThe filtrate was concentrated
  4. additionabsolute ethanol was added
  5. customevaporated
  6. additionether (100 ml) was added slowly
  7. customThe precipitate which formed
  8. customwas collected
  9. customdried in the air

출처 및 근거

ORD 기록
ord-31dbfbf0d2d845288c6f33f8219b38a0
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05929085

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