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Ethyl Acetate → HCID 22405461, 화합물

HRID 441215
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HRID 441215 반응식
FC(F)(F)[C:3]([N:5]([C:7]1[C:8](=[O:33])[N:9]([CH2:19][C:20]([NH:22][CH:23]([CH:30]([CH3:32])[CH3:31])[C:24](=[O:29])[C:25]([F:28])([F:27])[F:26])=[O:21])[C:10]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:11][CH:12]=1)C)=O.C(OCC)(=O)C>[Cl-].[Na+].O>[CH3:3][NH:5][C:7]1[C:8](=[O:33])[N:9]([CH2:19][C:20]([NH:22][CH:23]([CH:30]([CH3:31])[CH3:32])[C:24](=[O:29])[C:25]([F:26])([F:27])[F:28])=[O:21])[C:10]([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)=[CH:11][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8857Ethyl AcetateHCID 22405488HCID 22405488, 화합물

생성물 1

HCID 22405461HCID 22405461, 화합물

시약·촉매·용매 1

HCID 57417360Sodium chloride; water용매

실험 절차

Using a procedure similar to that described above under Example 49.j. for the basic hydrolysis of the analogous 3-(N-trifluoroacetylamino) compound to the 3-amino-compound, but using the following extractive work-up, the title compound was prepared from 2-[3-(N-trifluoroacetyl-N-methylamino)-2-oxo-6-phenyl -1,2-dihydro-1-pyridyl]-N-(3,3,3-trifluoro-1-isopropyl -2-oxopropyl)acetamide. On completion of hydrolysis, ethyl acetate and brine were added. The organic phase was separated, washed (brine), dried (MgSO4), and evaporated. The resultant solid was triturated with diethyl ether, chromatographed, eluting with dichloromethane:methanol (96:4), and dried overnight under vacuum to give the title product as a white solid; TLC: Rf =0.20, dichloromethane:methanol (96:4); MS: m/z=410(M+1).

후처리

  1. additionwere added
  2. customThe organic phase was separated
  3. washwashed (brine)
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. customThe resultant solid was triturated with diethyl ether
  7. customchromatographed
  8. washeluting with dichloromethane:methanol (96:4)
  9. customdried overnight under vacuum

출처 및 근거

ORD 기록
ord-a829f94132434107b3f6fdcc7153695e
출처 데이터셋
uspto-grants-1996_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05521179

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