Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 1-Propanesulfonyl chloride, 2-methyl- | HCID 182236 | — |
| Edukt | HCID 86675027 | HCID 86675027 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 86675029 | HCID 86675029 | 71% |
Reaktionsschritte
479 mg (3.0 mmol) of 2-methylpropane-1-sulfonyl chloride are added to a solution of 800 mg (2.8 mmol) of methyl (S)-3-tert-butoxycarbonylamino-2-piperazin-1-ylpropanoate (prepared as described in example 23.1) and 775 μl (5.5 mmol) of triethylamine in 8 ml of dichloromethane, cooled beforehand to 0° C. The reaction medium is stirred at ambient temperature for 18 h and then water is added and the medium is extracted with dichloromethane. The organic phase is washed with water, dried over magnesium sulfate, filtered and concentrated. The residue obtained is purified by chromatography on silica gel, elution being carried out with a 5/5 heptane/ethyl acetate mixture. 785 mg (71%) of methyl (S)-3-tert-butoxycarbonylamino-2-[4-(2-methylpropane-1-sulfonyl)piperazin-1-yl]propanoate are obtained in the form of a colorless oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08633196B2 |
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| Quelldatensatz | uspto-grants-2014_01 |
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| ORD ID | ord-a66e019be2004757ba6099e8750921a3 |
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| Quellennotiz | uspto-grants-2014_01 |
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