Hydrochloric Acid → 1-[1-(4-Pyridyl)-4-piperidinylamino]-2-piperazinone trihydrochloride

HRID 2086235노트

반응식

HRID 2086235 반응식
C(OC([N:11]1[CH2:16][CH2:15][N:14]([NH:17][CH:18]2[CH2:23][CH2:22][N:21]([C:24]3[CH:29]=[CH:28][N:27]=[CH:26][CH:25]=3)[CH2:20][CH2:19]2)[C:13](=[O:30])[CH2:12]1)=O)C1C=CC=CC=1.[ClH:31]>C(OCC)(=O)C.CO.[Pd]>[ClH:31].[ClH:31].[ClH:31].[N:27]1[CH:28]=[CH:29][C:24]([N:21]2[CH2:20][CH2:19][CH:18]([NH:17][N:14]3[CH2:15][CH2:16][NH:11][CH2:12][C:13]3=[O:30])[CH2:23][CH2:22]2)=[CH:25][CH:26]=1

참가 물질

6

반응물 2

HCID 313Hydrochloric AcidHCID 178254544-Benzyloxycarbonyl-1-[1-(4-pyridyl)-4-piperidinylamino]-2-piperazinone

생성물 1

HCID 695456121-[1-(4-Pyridyl)-4-piperidinylamino]-2-piperazinone trihydrochloride

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of 4-benzyloxycarbonyl-1-[1-(4-pyridyl)-4-piperidinylamino]-2-piperazinone (25.29 g) and an a 4N solution of hydrochloric acid in ethyl acetate (15.5 ml) in methanol (300 ml) was combined with 10% Pd/C (50% hydrated, 5.00 g) and stirred at room temperature for 15 hours under a hydrogen atmosphere. The catalyst was filtered off, and the reaction mixture was concentrated. The residue was dissolved in ethanol (300 ml), and combined with a 4N solution of hydrochloric acid in ethyl acetate (31 ml). The crystals precipitated were collected by filtration and dried to obtain 1-[1-(4-pyridyl)-4-piperidinylamino]-2-piperazinone trihydrochloride (20.16 g) as colorless crystals.

후처리

  1. filtrationThe catalyst was filtered off
  2. concentrationthe reaction mixture was concentrated
  3. dissolutionThe residue was dissolved in ethanol (300 ml)
  4. customThe crystals precipitated
  5. filtrationwere collected by filtration
  6. customdried

출처 및 근거

ORD 기록
ord-0d55b9eb262941a982003bef791d5c1f
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06723722B1

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