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2-Propanol, reaction products with ammonia, distn. residues → 5-(3-chlorophenyl)-alpha-(1-methyl-1H-imidazol-5-yl)-alpha-(4-methylphenyl)-tetrazolo[1,5-a]quinazoline-7-methanamine hydrate

HRID 1788065
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HRID 1788065 반응식
Cl.Cl[C:3]([C:31]1[N:35]([CH3:36])[CH:34]=[N:33][CH:32]=1)([C:24]1[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][CH:25]=1)[C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[N:10]1[N:14]=[N:15][N:16]=[C:9]1[N:8]=[C:7]2[C:17]1[CH:22]=[CH:21][CH:20]=[C:19]([Cl:23])[CH:18]=1.[NH3:37].CC([OH:41])C>C1COCC1>[OH2:41].[Cl:23][C:19]1[CH:18]=[C:17]([C:7]2[C:6]3[C:11](=[CH:12][CH:13]=[C:4]([C:3]([C:31]4[N:35]([CH3:36])[CH:34]=[N:33][CH:32]=4)([C:24]4[CH:25]=[CH:26][C:27]([CH3:30])=[CH:28][CH:29]=4)[NH2:37])[CH:5]=3)[N:10]3[N:14]=[N:15][N:16]=[C:9]3[N:8]=2)[CH:22]=[CH:21][CH:20]=1
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참가 물질

4

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HCID 183319422-Propanol, reaction products with ammonia, distn. residuesHCID 1317273757-[chloro(1-methyl-1H-imidazol-5-yl)(4-methylphenyl)methyl]-5-(3-chlorophenyl)-tetrazolo[1,5-a]quinazoline. hydrochloride

생성물 1

HCID 688609215-(3-chlorophenyl)-alpha-(1-methyl-1H-imidazol-5-yl)-alpha-(4-methylphenyl)-tetrazolo[1,5-a]quinazoline-7-methanamine hydrate수율 33%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

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온도
5 °C

실험 절차

A mixture of intermediate 26 (0.0083 mol) in THF (80 ml) was cooled to 5° C. under N2 flow. NH3/iPrOH (80 ml) was added dropwise. The mixture was stirred at 5° C. for 1 hours, then brought to room temperature. The mixture was stirred at room temperature overnight, poured out into ice water and extracted with DCM. The organic layer was separated, washed with water, dried (MgSO4), filtered and the solvent was evaporated. The residue was purified by column chromatography over silica gel (15-40 μm) (eluent: DCM/MeOH/NH4OH 96/4/0.2). The pure fractions were collected and the solvent was evaporated. The residue was crystallized from CH3CN. The precipitate was filtered off and dried, yielding 1.37 g (33%) of 5-(3-chlorophenyl)-α-(1-methyl-1H-imidazol-5-yl)-α-(4-methylphenyl)-tetrazolo[1,5-a]quinazoline-7-methanamine hydrate (1:1) (intermediate 27), mp. 150° C.

후처리

  1. custombrought to room temperature
  2. stirringThe mixture was stirred at room temperature overnight
  3. extractionextracted with DCM
  4. customThe organic layer was separated
  5. washwashed with water
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. customthe solvent was evaporated
  9. customThe residue was purified by column chromatography over silica gel (15-40 μm) (eluent: DCM/MeOH/NH4OH 96/4/0.2)
  10. customThe pure fractions were collected
  11. customthe solvent was evaporated
  12. customThe residue was crystallized from CH3CN
  13. filtrationThe precipitate was filtered off
  14. customdried

출처 및 근거

ORD 기록
ord-a3801d7d96d54cd2841fea0fa8ce85b6
출처 데이터셋
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07511138B2

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