Hydrochloric Acid → 1-Amino-4-(3-methoxy-phenyl)-pyrrolidin-2-one

HRID 8203ノート

反応式

HRID 8203 の反応式
Cl.C(=[N:15][N:16]1[CH2:20][CH:19]([C:21]2[CH:26]=[CH:25][CH:24]=[C:23]([O:27][CH3:28])[CH:22]=2)[CH2:18][C:17]1=[O:29])(C1C=CC=CC=1)C1C=CC=CC=1>O>[NH2:15][N:16]1[CH2:20][CH:19]([C:21]2[CH:26]=[CH:25][CH:24]=[C:23]([O:27][CH3:28])[CH:22]=2)[CH2:18][C:17]1=[O:29]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 219926151-(Benzhydrylidene-amino)-4-(3-methoxy-phenyl)-pyrrolidin-2-one

生成物 1

HCID 219926971-Amino-4-(3-methoxy-phenyl)-pyrrolidin-2-one

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Concentrated hydrochloric acid (0.35 mL) is added to a suspension of 1-(benzhydrylidene-amino)-4-(3-methoxy-phenyl)-pyrrolidin-2-one, (0.8 g, 2.16 mmol) in water (17 mL) and refluxed for one hour. The mixture is concentrated in vacuo and water azeotroped away using ethanol and toluene. The residue is dissolved in methanol (5 mL) and loaded on SCX resin (5 g). The resin is washed with methanol and 2 M solution of ammonia in methanol. Appropriate fractions are concentrated to yield the title compound, 402 mg (92%), as a white crystalline solid.

後処理

  1. temperaturerefluxed for one hour
  2. concentrationThe mixture is concentrated in vacuo and water
  3. customazeotroped away using ethanol and toluene
  4. dissolutionThe residue is dissolved in methanol (5 mL)
  5. washThe resin is washed with methanol and 2 M solution of ammonia in methanol
  6. concentrationAppropriate fractions are concentrated

出典と根拠

ORDレコード
ord-ea0419dad2e9469f94ef59108d4767eb
出典データセット
uspto-grants-2006_08
特許番号
US07087626B2

反応ノート

読み込み中…