Hydrochloric Acid → N-(4-Fluoro-3-chloro-phenyl)-2-[N-methyl-N-(2,2-difluoroethyl)-amino]-4-methylamino-5-nitro-benzoic acid amide

HRID 1189633Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1189633
[F:1][CH:2]([F:6])[CH2:3][NH:4][CH3:5].Cl.CCN(C(C)C)C(C)C.[F:17][C:18]1[CH:23]=[CH:22][C:21]([NH:24][C:25](=[O:38])[C:26]2[CH:31]=[C:30]([N+:32]([O-:34])=[O:33])[C:29]([NH:35][CH3:36])=[CH:28][C:27]=2F)=[CH:20][C:19]=1[Cl:39]>CC#N>[F:17][C:18]1[CH:23]=[CH:22][C:21]([NH:24][C:25](=[O:38])[C:26]2[CH:31]=[C:30]([N+:32]([O-:34])=[O:33])[C:29]([NH:35][CH3:36])=[CH:28][C:27]=2[N:4]([CH3:5])[CH2:3][CH:2]([F:6])[F:1])=[CH:20][C:19]=1[Cl:39]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 81531DiisopropylethylamineHCID 233232502,2-difluoro-N-methylethanamineHCID 67957648N-(4-Fluoro-3-chloro-phenyl)-2-fluoro-4-methylamino-5-nitro-benzoic acid amide

Produkt 1

HCID 86666463N-(4-Fluoro-3-chloro-phenyl)-2-[N-methyl-N-(2,2-difluoroethyl)-amino]-4-methylamino-5-nitro-benzoic acid amide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A mixture of N-(2,2-difluoroethyl)-N-methyl-amine×HCl (64 mg, 0.48 mmol), DIPEA (0.64 ml, 3.73 mmol), N-(4-fluoro-3-chloro-phenyl)-2-fluoro-4-methylamino-5-nitro-benzoic acid amide (150 mg, 0.44 mmol) and MeCN (5 mL) is stirred for two weeks at reflux. Then the mixture is concentrated, diluted with EtOAc, washed with water, dried with Na2SO4 and concentrated and directly used in the next step.

Aufarbeitung

  1. temperatureat reflux
  2. concentrationThen the mixture is concentrated
  3. additiondiluted with EtOAc
  4. washwashed with water
  5. dry with materialdried with Na2SO4
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-95e76a4fbdac4df9a635710c329bcbf1
Quelldatensatz
uspto-grants-2014_03
Patentnummer
US08674113B2

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