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Trifluoroacetic acid → HCID 57671538, 화합물

HRID 1801990
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HRID 1801990 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]([NH:12][CH3:13])=[CH:10][N:11]=1)[C:5]([O:7]C)=O.[C:14]([O:18][C:19]([C:21]1[C:26](C(OC)=O)=CC(Cl)=NC=1)=[O:20])(C)(C)C.C(O)(C(F)(F)F)=[O:33]>C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][N:11]=1)[N:12]([CH3:13])[C:26](=[O:33])[C:21]([C:19]([O:18][CH3:14])=[O:20])=[C:5]2[OH:7]
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참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 57671617HCID 57671617, 화합물HCID 86631269HCID 86631269, 화합물

생성물 1

HCID 57671538HCID 57671538, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Methyl 2-chloro-5-(methylamino)isonicotinate. To a solution of methyl 5-(tert-butoxycarbonyl)-2-chloroisonicotinate (0.5 g, 1.7 mmol) in dry DCM (10 mL) was added TFA (4.4 mL) with stirring and cooling using an ice-bath. The mixture was stirred at room temperature for 2 hours and then evaporated under reduced pressure. The residue was dissolved in water, and the solution was adjusted to pH=8 by treatment with saturated NaHCO3. The mixture was extracted twice with EtOAc. The combined organic layers were dried over anhydrous MgSO4, and filtered. The filtrate was evaporated under reduced pressure, and the residue was dried in vacuo to give the title compound.

후처리

  1. temperaturecooling
  2. stirringThe mixture was stirred at room temperature for 2 hours
  3. customevaporated under reduced pressure
  4. dissolutionThe residue was dissolved in water
  5. extractionThe mixture was extracted twice with EtOAc
  6. dry with materialThe combined organic layers were dried over anhydrous MgSO4
  7. filtrationfiltered
  8. customThe filtrate was evaporated under reduced pressure
  9. customthe residue was dried in vacuo

출처 및 근거

ORD 기록
ord-f27b3c908d9f455395190c591d0e0a4c
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08349868B2

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