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Hydrochloric Acid → Ethyl 1-(2,4-difluorophenyl)-6-fluoro-1,4-dihydro-4-oxo-7-(2,4,6-trimethylbenzenesulfonyloxy)-1,8-naphthyridine-3-carboxylate

HRID 232479
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 232479
[CH3:1]N(C)C=O.S(OC)(OC)(=O)=O.C[O-].[Na+].[F:16][C:17]1[CH:22]=[C:21]([F:23])[CH:20]=[CH:19][C:18]=1[NH:24][C:25]1[N:38]=[C:37]([O:39][S:40]([C:43]2[C:48]([CH3:49])=[CH:47][C:46]([CH3:50])=[CH:45][C:44]=2[CH3:51])(=[O:42])=[O:41])[C:36]([F:52])=[CH:35][C:26]=1[C:27]([CH2:29][C:30]([O:32][CH2:33][CH3:34])=[O:31])=[O:28].C(OC(=O)C)(=O)C.Cl.C(OC(C)C)(C)C>O.C(Cl)Cl.C(O)C>[F:16][C:17]1[CH:22]=[C:21]([F:23])[CH:20]=[CH:19][C:18]=1[N:24]1[C:25]2[C:26](=[CH:35][C:36]([F:52])=[C:37]([O:39][S:40]([C:43]3[C:48]([CH3:49])=[CH:47][C:46]([CH3:50])=[CH:45][C:44]=3[CH3:51])(=[O:41])=[O:42])[N:38]=2)[C:27](=[O:28])[C:29]([C:30]([O:32][CH2:33][CH3:34])=[O:31])=[CH:1]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

10

Edukt 6

HCID 313Hydrochloric AcidHCID 7914Diisopropyl EtherHCID 7918Acetic AnhydrideHCID 10942334Sodium MethoxideHCID 11127270DMF dimethylsulfateHCID 13849317Ethyl 2-[2-(2,4-difluorophenylamino)-5-fluoro-6-(2,4,6-trimethylbenzenesulfonyloxy)nicotinoyl]acetate

Produkt 1

HCID 13849332Ethyl 1-(2,4-difluorophenyl)-6-fluoro-1,4-dihydro-4-oxo-7-(2,4,6-trimethylbenzenesulfonyloxy)-1,8-naphthyridine-3-carboxylateAusbeute 80,2 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittelHCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To 6 ml of methylene chloride was added 335 mg of (N,N-dimethylformamide-dimethyl sulfate) complex compound, and 65 mg of sodium methoxide was added thereto at 0° C., after which the resulting mixture was subjected to reaction at 0° to 10° C. for 1 hour. Subsequently, 300 mg of ethyl 2-[2-(2,4-difluorophenylamino)-5-fluoro-6-(2,4,6-trimethylbenzenesulfonyloxy)nicotinoyl]acetate and 115 mg of acetic anhydride were added thereto. The resulting mixture was subjected to reaction at room temperature for 2 hours, and 0.31 ml of 2N hydrochloric acid and 3 ml of ethanol were added to the reaction mixture, after which the resulting mixture was subjected to reaction at room temperature for 1.5 hours. The reaction mixture was added to a mixture of 6 ml of methylene chloride and 6 ml of water, and the organic layer was separated, washed with 6 ml of saturated aqueous sodium chloride solution, and then dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure, and to the crystalline material thus obtained was added 2 ml of diisopropyl ether, after which crystals were collected by filtration to obtain 245 mg (yield 80.2%) of ethyl 1-(2,4-difluorophenyl)-6-fluoro-1,4-dihydro-4-oxo-7-(2,4,6-trimethylbenzenesulfonyloxy)-1,8-naphthyridine-3-carboxylate. The physical properties of this compound were identical with those of the compound obtained in Example 41.

Aufarbeitung

  1. additionwas added
  2. customat 0° C., after which the resulting mixture was subjected to reaction at 0° to 10° C. for 1 hour
  3. customThe resulting mixture was subjected to reaction at room temperature for 2 hours
  4. customafter which the resulting mixture was subjected to reaction at room temperature for 1.5 hours
  5. customthe organic layer was separated
  6. washwashed with 6 ml of saturated aqueous sodium chloride solution
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customThe solvent was removed by distillation under reduced pressure
  9. customto the crystalline material thus obtained
  10. filtrationafter which crystals were collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-3a6e0767c75d4cd1aedc2edb20742a9c
Quelldatensatz
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04851535

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