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Ammonium formate → HCID 22144666, 화합물

HRID 1824979
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HRID 1824979 반응식
[F:1][C:2]1[CH:30]=[C:29]([F:31])[CH:28]=[CH:27][C:3]=1[CH2:4][N:5]1[C:13]2[C:8](=[CH:9][C:10]([N+:14]([O-])=O)=[CH:11][CH:12]=2)[CH:7]=[C:6]1[C:17]([NH:19][C:20]1[CH:25]=[CH:24][C:23]([F:26])=[CH:22][CH:21]=1)=[O:18].C([O-])=O.[NH4+]>C(OCC)(=O)C.C(O)C.[Pd]>[NH2:14][C:10]1[CH:9]=[C:8]2[C:13](=[CH:12][CH:11]=1)[N:5]([CH2:4][C:3]1[CH:27]=[CH:28][C:29]([F:31])=[CH:30][C:2]=1[F:1])[C:6]([C:17]([NH:19][C:20]1[CH:25]=[CH:24][C:23]([F:26])=[CH:22][CH:21]=1)=[O:18])=[CH:7]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 2723923Ammonium formate2회HCID 22144644HCID 22144644, 화합물

생성물 1

HCID 22144666HCID 22144666, 화합물

시약·촉매·용매 3

HCID 23938Palladium촉매2회HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

실험 절차

485 mg (1.14 mmol) of 1-(2,4-difluorobenzyl)-N-(4-fluorophenyl)-5-nitro-1H-indole-2-carboxamide from Example XXIV are initially charged in ethyl acetate and ethanol. 287 mg (4.56 mmol) of ammonium formate and 49 mg of palladium on activated carbon (10%) are added. The mixture is heated to reflux, and at 50° C. gas evolves. To bring the reaction to completion, the same amounts of ammonium formate and palladium as above are added. After a further 3 hours at reflux, the mixture is cooled and filtered off through kieselguhr, which is washed with 500 ml of ethanol. The solvent is removed under reduced pressure and the residue is dried.

후처리

  1. temperatureThe mixture is heated
  2. temperatureto reflux
  3. customat 50° C.
  4. customthe reaction to completion
  5. temperatureAfter a further 3 hours at reflux
  6. temperaturethe mixture is cooled
  7. filtrationfiltered off through kieselguhr, which
  8. washis washed with 500 ml of ethanol
  9. customThe solvent is removed under reduced pressure
  10. customthe residue is dried

출처 및 근거

ORD 기록
ord-378d339d207348419f28bbc049321e5a
출처 데이터셋
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07045544B2

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