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HCID 70574680、化合物 → 2-[(4-methoxyphenyl)methyl]pyrrolidine

HRID 1278037
ノート
印刷プレビュー

反応式

HRID 1278037 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 70574680HCID 70574680、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

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).

後処理

custom
the 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
  • 出典と根拠

    ORDレコード
    ord-61357ace7ab640d18f12334116565d3e
    出典データセット
    uspto-grants-1981_07
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US04279918

    反応ノート

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