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HCID 70574680, 화합물 → 2-[(4-methoxyphenyl)methyl]pyrrolidine

HRID 1278037
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HRID 1278037 반응식
C(OC([C:8](=[C:17]1[CH2:21][CH2:20][CH2:19][NH:18]1)[C:9]1[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=1)=O)(C)(C)C>FC(F)(F)C(O)=O>[CH3:16][O:15][C:12]1[CH:11]=[CH:10][C:9]([CH2:8][CH:17]2[CH2:21][CH2:20][CH2:19][NH:18]2)=[CH:14][CH:13]=1
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참가 물질

3

반응물 1

HCID 70574680HCID 70574680, 화합물

생성물 1

HCID 49955292-[(4-methoxyphenyl)methyl]pyrrolidine

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

Add 80 ml of trifluoroacetic acid to 15 g of the title compound of Example 17 with ice cooling, and stir the produced reaction mixture for 2 hours at room temperature. Distil off the acid under a vacuum. Dissolve the resulting residue in 250 ml of diethyl ether and wash the thus-prepared solution with almost saturated cold sodium carbonate solution (150 ml) and saturated sodium chloride solution. Dry the washed solution over sodium sulfate and distil off the ether before dissolving the residue in 300 ml of ethanol and reducing it with Raney nickel/hydrogen. Concentrate the reduced solution to an oil and distil the oil under a vacuum to obtain 7.5 g (76% of theory) of the title compound (b.p. 88° to 90° at 0.008 mm of Hg).

후처리

  • customthe produced reaction mixture for 2 hours at room temperature
  • customDistil off the acid under a vacuum
  • dissolutionDissolve the resulting residue in 250 ml of diethyl ether
  • washwash the thus-prepared solution with almost saturated cold sodium carbonate solution (150 ml) and saturated sodium chloride solution
  • dry with materialDry the washed solution over sodium sulfate
  • customdistil off the ether
  • dissolutionbefore dissolving the residue in 300 ml of ethanol
  • concentrationConcentrate the reduced solution to an oil
  • customdistil the oil under a vacuum
  • 출처 및 근거

    ORD 기록
    ord-61357ace7ab640d18f12334116565d3e
    출처 데이터셋
    uspto-grants-1981_07
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04279918

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