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2,4-Dichlorobenzylamine → N-(2,4-Dichlorobenzyl)-7-[(3RS,5RS)-3,5-dimethylpiperazin-1-yl]-6-fluoro-8-methoxy-1-(2,2,2-trifluoroethyl)-4-oxo-1,4-dihydroquinoline-3-carboxamide

HRID 2099315
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2099315
C(N(CC)C(C)C)(C)C.C1CN([P+](ON2N=NC3C=CC=CC2=3)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F.[CH3:43][C@H:44]1[NH:49][C@@H:48]([CH3:50])[CH2:47][N:46]([C:51]2[C:60]([O:61][CH3:62])=[C:59]3[C:54]([C:55](=[O:71])[C:56]([C:68](O)=[O:69])=[CH:57][N:58]3[CH2:63][C:64]([F:67])([F:66])[F:65])=[CH:53][C:52]=2[F:72])[CH2:45]1.[Cl:73][C:74]1[CH:81]=[C:80]([Cl:82])[CH:79]=[CH:78][C:75]=1[CH2:76][NH2:77].C(#N)C>CN(C)C=O.C(OCC)(=O)C>[Cl:73][C:74]1[CH:81]=[C:80]([Cl:82])[CH:79]=[CH:78][C:75]=1[CH2:76][NH:77][C:68]([C:56]1[C:55](=[O:71])[C:54]2[C:59](=[C:60]([O:61][CH3:62])[C:51]([N:46]3[CH2:45][CH:44]([CH3:43])[NH:49][CH:48]([CH3:50])[CH2:47]3)=[C:52]([F:72])[CH:53]=2)[N:58]([CH2:63][C:64]([F:66])([F:67])[F:65])[CH:57]=1)=[O:69]
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Komponenten

8

Edukt 5

HCID 14852,4-DichlorobenzylamineHCID 6342AcetonitrileHCID 81531DiisopropylethylamineHCID 2724699PyBOPHCID 577941837-(cis-3,5-Dimethylpiperazin-1-yl)-6-fluoro-8-methoxy-1-(2,2,2-trifluoroethyl)-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

Produkt 1

HCID 76607220
N-(2,4-Dichlorobenzyl)-7-[(3RS,5RS)-3,5-dimethylpiperazin-1-yl]-6-fluoro-8-methoxy-1-(2,2,2-trifluoroethyl)-4-oxo-1,4-dihydroquinoline-3-carboxamide
Ausbeute 0,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Under argon, 7.52 g (58.2 mmol) of N,N-diisopropylethylamine and 7.71 g (14.81 mmol) of PyBOP are added to 5.20 g (10.58 mmol) of 7-(cis-3,5-dimethylpiperazin-1-yl)-6-fluoro-8-methoxy-1-(2,2,2-trifluoroethyl)-4-oxo-1,4-dihydroquinoline-3-carboxylic acid hydroformate (Example 31A) and 3.73 g (21.2 mmol) of 2,4-dichlorobenzylamine in 10.7 ml of dimethylformamide and the mixture is stirred at room temperature overnight. The reaction mixture is diluted with 1500 ml of ethyl acetate and washed three times with water. The combined aqueous phases are extracted once with ethyl acetate. The combined organic phases are washed with a saturated sodium chloride solution, dried over sodium sulfate and concentrated. The residue is stirred with 30 ml of acetonitrile. The solid is then collected by filtration and dried under high vacuum. 6.80 mg of the target compound are obtained as a cocrystallisate with 1 eq. of acetonitrile. For smaller quantities the residue after extraction can be purified by preparative HPLC (by one of the methods 5 to 8).

Aufarbeitung

  1. washwashed three times with water
  2. extractionThe combined aqueous phases are extracted once with ethyl acetate
  3. washThe combined organic phases are washed with a saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. stirringThe residue is stirred with 30 ml of acetonitrile
  7. filtrationThe solid is then collected by filtration
  8. customdried under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-405ae29eece54f16b64592e028ce1f0f
Quelldatensatz
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07569563B2

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