Hydrochloric Acid → alpha-Phenyl-1-[4-[[[4'-(trifluoromethyl)[1,1'-biphenyl]-2-yl]carbonyl]amino]phenyl]-4-piperidineacetic acid monohydrochloride

HRID 1989867노트

반응식

HRID 1989867 반응식
[C:1]1([CH:7]([CH:12]2[CH2:17][CH2:16][N:15]([C:18]3[CH:23]=[CH:22][C:21]([NH:24][C:25]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=4[C:33]4[CH:38]=[CH:37][C:36]([C:39]([F:42])([F:41])[F:40])=[CH:35][CH:34]=4)=[O:26])=[CH:20][CH:19]=3)[CH2:14][CH2:13]2)[C:8]([O:10]C)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.[ClH:44]>O1CCOCC1>[ClH:44].[C:1]1([CH:7]([CH:12]2[CH2:13][CH2:14][N:15]([C:18]3[CH:23]=[CH:22][C:21]([NH:24][C:25]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=4[C:33]4[CH:38]=[CH:37][C:36]([C:39]([F:42])([F:40])[F:41])=[CH:35][CH:34]=4)=[O:26])=[CH:20][CH:19]=3)[CH2:16][CH2:17]2)[C:8]([OH:10])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 22499403Methyl alpha-phenyl-1-[4-[[[4'-(trifluoromethyl)-[1,1'-biphenyl]-2-yl]carbonyl]amino]phenyl]-4-piperidineacetate

생성물 1

HCID 68521936alpha-Phenyl-1-[4-[[[4'-(trifluoromethyl)[1,1'-biphenyl]-2-yl]carbonyl]amino]phenyl]-4-piperidineacetic acid monohydrochloride

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of intermediate (23) (0.0014 mol) in concentrated HCl (25 ml) and dioxane (20 ml) was stirred and refluxed for 4 hours, cooled and poured out into water. The mixture was extracted with DCM. The organic layer was separated, dried, filtered and the solvent was evaporated. The residue was triturated in DIPE. The precipitate was filtered off and dried, yielding 0.48 g of α-phenyl-1-[4-[[[4′-(trifluoromethyl)[1,1′-biphenyl]-2-yl]carbonyl]amino]phenyl]-4-piperidineacetic acid monohydrochloride (intermediate 24, mp. 196° C.).

후처리

  1. temperaturerefluxed for 4 hours
  2. temperaturecooled
  3. extractionThe mixture was extracted with DCM
  4. customThe organic layer was separated
  5. customdried
  6. filtrationfiltered
  7. customthe solvent was evaporated
  8. customThe residue was triturated in DIPE
  9. filtrationThe precipitate was filtered off
  10. customdried

출처 및 근거

ORD 기록
ord-c125aa466ef14ef88ea4d13d20f8f737
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07642378B2

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