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

HRID 8203노트

반응식

HRID 8203 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ea0419dad2e9469f94ef59108d4767eb
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07087626B2

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