Ethanol → Caspofungin Acetate

HRID 2173738Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2173738
[CH3:1][CH2:2][CH:3]([CH2:5][CH:6]([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]([NH:18][C@@H:19]1[C:50](=[O:51])[NH:49][C@@H:48]([C@H:52]([OH:54])[CH3:53])[C:46](=[O:47])[N:45]2[C@@H:41]([CH2:42][C@@H:43]([OH:55])[CH2:44]2)[C:39](=[O:40])[NH:38][C@@H:37]([C@H:56]([OH:66])[C@@H:57]([OH:65])[C:58]2[CH:59]=[CH:60][C:61]([OH:64])=[CH:62][CH:63]=2)[C:35](=[O:36])[NH:34][C@@H:33]([C@H:67]([OH:71])[CH2:68][CH2:69][NH2:70])[C:31](=[O:32])[N:30]2[C@@H:26]([C@@H:27]([OH:72])[CH2:28][CH2:29]2)[C:24](=[O:25])[NH:23][C@H:22]([NH:73][CH2:74][CH2:75][NH2:76])[C@H:21]([OH:77])[CH2:20]1)=[O:17])[CH3:7])[CH3:4].C(O)C.[C:81]([O:84]CC)(=[O:83])[CH3:82].N[C@H:88]([C:97]([OH:99])=[O:98])CC1C=CC(O)=CC=1>CO[2H].C(O)(=O)C>[CH3:1][CH2:2][CH:3]([CH2:5][CH:6]([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]([NH:18][C@@H:19]1[C:50](=[O:51])[NH:49][C@@H:48]([C@H:52]([OH:54])[CH3:53])[C:46](=[O:47])[N:45]2[C@@H:41]([CH2:42][C@@H:43]([OH:55])[CH2:44]2)[C:39](=[O:40])[NH:38][C@@H:37]([C@H:56]([OH:66])[C@@H:57]([OH:65])[C:58]2[CH:59]=[CH:60][C:61]([OH:64])=[CH:62][CH:63]=2)[C:35](=[O:36])[NH:34][C@@H:33]([C@H:67]([OH:71])[CH2:68][CH2:69][NH2:70])[C:31](=[O:32])[N:30]2[C@@H:26]([C@@H:27]([OH:72])[CH2:28][CH2:29]2)[C:24](=[O:25])[NH:23][C@H:22]([NH:73][CH2:74][CH2:75][NH2:76])[C@H:21]([OH:77])[CH2:20]1)=[O:17])[CH3:7])[CH3:4].[CH3:82][C:81]([OH:84])=[O:83].[CH3:88][C:97]([OH:99])=[O:98]

Komponenten

7

Edukt 4

HCID 702EthanolHCID 6057L-TyrosineHCID 8857Ethyl AcetateHCID 2826718n-{(2r,6s,9s,11r,12s,14As,15s,20s,23s,25as)-12-[(2-aminoethyl)amino]-20-[(1r)-3-amino-1-hydroxypropyl]-23-[(1s,2s)-1,2-dihydroxy-2-(4-hydroxyphenyl)ethyl]-2,11,15-trihydroxy-6-[(1r)-1-hydroxyethyl]-5,8,14,19,22,25-hexaoxotetracosahydro-1h-dipyrrolo[2,1-c:2',1'-l][1,4,7,10,13,16]hexaazacyclohenicosin-9-yl}-10,12-dimethyltetradecanamide2×

Produkt 1

HCID 6850808Caspofungin Acetate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 123113Methan(2H)olLösungsmittel

Versuchsvorschrift

By means of NMR the contents of caspofungin, ethanol, ethyl acetate and acetic acid were determined in the crystals obtained above as follows. Approximately 15 mg of sample and standard (DMB) were accurately weighed in a suitable vial. The samples were dissolved in MeOD by vortexing. The samples were measured at 600 MHz using a delay of 30 s at 300K. The spectra that were used for the calculation of the impurities in the aromatic region were measured using a delay of 5 s and 256 scans to enhance the signal to noise ratio. The analysis was carried out in duplo. Caspofungin was quantified using the tyrosine signal at 7.15 ppm. See Table 5 for results.

Aufarbeitung

  1. customobtained above
  2. customfor results

Quellen und Nachweise

ORD-Eintrag
ord-e39fd8ca65ae4faeabc33b9378de8bba
Quelldatensatz
uspto-grants-2015_06
Patentnummer
US09056897B2

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