化工社化工社 化学情報印刷レポート · 研究参考用
Ethanol → Caspofungin Acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | L-Tyrosine | HCID 6057 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | n-{(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-dimethyltetradecanamide | HCID 2826718 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Methan(2H)ol | HCID 123113 | — |
| 生成物 | Caspofungin Acetate | HCID 6850808 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09056897B2 |
| 出典データセット | uspto-grants-2015_06 |
| ORD ID | ord-e39fd8ca65ae4faeabc33b9378de8bba |
| 出典メモ | uspto-grants-2015_06 |