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Hydrochloric Acid → 5-methyl-2-(4-piperidinyl)methyl-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one dihydrochloride

HRID 1162328
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HRID 1162328 반응식
[CH3:1][C:2]1[N:6]2[C:7](=[O:24])[N:8]([CH2:10][CH:11]3[CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][CH2:12]3)[CH2:9][C:5]2=[CH:4][N:3]=1.[ClH:25]>C(O)C>[ClH:25].[ClH:25].[CH3:1][C:2]1[N:6]2[C:7](=[O:24])[N:8]([CH2:10][CH:11]3[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]3)[CH2:9][C:5]2=[CH:4][N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 23138425tert-butyl 4-((5-methyl-3-oxo-1H-imidazo[1,5-c]imidazol-2(3H)-yl)methyl)-1-piperidinecarboxylate

생성물 1

HCID 231381375-methyl-2-(4-piperidinyl)methyl-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one dihydrochloride수율 78%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To tert-butyl 4-((5-methyl-3-oxo-1H-imidazo[1,5-c]imidazol-2(3H)-yl)methyl)-1-piperidinecarboxylate (3.5 g) obtained in Example 85a) was added concentrated hydrochloric acid (10 ml), and mixed for 10 minutes. To the reaction mixture was added ethanol, and the solvent was distilled off under reduced pressure. To the residue was further added ethanol, and the solvent was distilled off under reduced pressure. To the residue was added isopropyl alcohol, and the precipitate was collected by filtration. The precipitate was washed sequentially with isopropyl alcohol and diethyl ether and dried under reduced pressure to obtain 5-methyl-2-(4-piperidinyl)methyl-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one dihydrochloride as a colorless solid (2.5 g, 78%).

후처리

  1. additionmixed for 10 minutes
  2. distillationthe solvent was distilled off under reduced pressure
  3. distillationthe solvent was distilled off under reduced pressure
  4. additionTo the residue was added isopropyl alcohol
  5. filtrationthe precipitate was collected by filtration
  6. washThe precipitate was washed sequentially with isopropyl alcohol and diethyl ether
  7. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-3c01014afba649549ba72d67538716f5
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07820673B2

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