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

HRID 846179ノート

反応式

HRID 846179 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 113%

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 g 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-58482b7f57b24eb5be79ae3bef2a7912
出典データセット
uspto-grants-1992_08
特許番号
US05135944

反応ノート

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