Hydrochloric Acid → Pyrrolidine, 2-[(3,4-dimethoxyphenyl)methyl]-, (R)-

HRID 2372833ノート

反応式

HRID 2372833 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:18]=[CH:19][C:20]=1[O:21][CH3:22])[CH2:6][C@H:7]1[CH2:11][CH2:10][CH2:9][N:8]1C(=O)C(F)(F)F.Cl>C(O)(C)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:18]=[CH:19][C:20]=1[O:21][CH3:22])[CH2:6][C@H:7]1[CH2:11][CH2:10][CH2:9][NH:8]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 13330057HCID 13330057、化合物

生成物 1

HCID 11831008Pyrrolidine, 2-[(3,4-dimethoxyphenyl)methyl]-, (R)-収率 97%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

To a solution of (R)-2-(3,4-dimethoxybenzyl)-1-trifluoroacetylpyrrolidine (3.2 g, 0.010 mol) in 50 mL isopropyl alcohol was added 15 mL of 12.5M HCl. The mixture was then heated under reflux until all starting material had disappeared, approximately 24 hours. The solvent was removed in vacuo to give an oil which could be recrystallized from isopropyl alcohol/ether, giving 2.5 of (R)-2-(3,4-dimethoxybenzyl)pyrrolidine (97% yield), as needles, m.p. 165°-167° C.

後処理

  1. temperatureThe mixture was then heated
  2. temperatureunder reflux until all starting material
  3. customThe solvent was removed in vacuo
  4. customto give an oil which
  5. customcould be recrystallized from isopropyl alcohol/ether

出典と根拠

ORDレコード
ord-b0d519e2282c48aeb0053a70021d26b5
出典データセット
uspto-grants-1992_03
特許番号
US05100912

反応ノート

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