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Hydrochloric Acid → Spiro[indene-1,4'-piperidine] hydrochloride

HRID 1534785
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반응식

HRID 1534785 반응식
C(OC([N:8]1[CH2:13][CH2:12][C:11]2([C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:15]=[CH:14]2)[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:22]>C(OCC)(=O)C>[ClH:22].[NH:8]1[CH2:13][CH2:12][C:11]2([C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:15]=[CH:14]2)[CH2:10][CH2:9]1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 3653579Tert-butyl Spiro[indene-1,4'-piperidine]-1'-carboxylate

생성물 1

HCID 22509344Spiro[indene-1,4'-piperidine] hydrochloride

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

1'-(t-Butyloxycarbonyl)spiro(indene-1,4'-piperidine) (16 g, 56 mmole) in ethyl acetate (250 ml) was stirred in an ice bath and saturated with HCl(g) for 30 min. The mixture was evaporated to dryness. Ethyl acetate was added and removed in vacuo three times, and the residue was triturated with diethyl ether and filtered to provide spiro(1H-indene-1,4'-piperidine) hydrochloride. The free base was obtained by slurrying the hydrochloride in aqueous sodium bicarbonate solution and extracting with CH2Cl2. The organic layer was separated, dried over sodium sulfate, filtered, and evaporated to dryness in vacuo to provide the title compound.

후처리

  1. customThe mixture was evaporated to dryness
  2. additionEthyl acetate was added
  3. customremoved in vacuo three times
  4. customthe residue was triturated with diethyl ether
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-24ad0375c3c74e61bbc6e4a8e7e6473f
출처 데이터셋
uspto-grants-1992_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05091387

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