Ethanol → Caspofungin Acetate

HRID 2173738

反応式

HRID 2173738 の反応式
[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]

参加物

7

反応物 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 回

生成物 1

HCID 6850808Caspofungin Acetate

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 123113Methan(2H)ol溶媒

実験手順

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.

後処理

  1. customobtained above
  2. customfor results

出典と根拠

ORDレコード
ord-e39fd8ca65ae4faeabc33b9378de8bba
出典データセット
uspto-grants-2015_06
特許番号
US09056897B2

関連ノート

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