Ethanol → Caspofungin Acetate

HRID 2173738

반응식

HRID 2173738 반응식
[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]

참가 물질

7

반응물 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-dimethyltetradecanamide2회

생성물 1

HCID 6850808Caspofungin Acetate

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 123113Methan(2H)ol용매

실험 절차

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.

후처리

  1. customobtained above
  2. customfor results

출처 및 근거

ORD 기록
ord-e39fd8ca65ae4faeabc33b9378de8bba
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09056897B2

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