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HRID 80936Erstellt: 23. Oktober 2026
Hydrochloric Acid → 2-[4-(4-Isopropyl-3,4,5,6-tetrahydro-2H-[1,2']bipyrazinyl-5'-yl)phenoxy]-N,N-dimethylacetamide, dihydrochloride
https://huagongshe.com/de/reaction/80936
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 2-chloro-N,N-dimethylacetamide | HCID 75886 | — |
| Edukt | HCID 136099407 | HCID 136099407 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 2-[4-(4-Isopropyl-3,4,5,6-tetrahydro-2H-[1,2']bipyrazinyl-5'-yl)phenoxy]-N,N-dimethylacetamide, dihydrochloride | HCID 131730786 | 41% |
Reaktionsschritte
4-(4-Isopropyl-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl-5′-yl)phenol (0.15 g, 0.404 mmol) was dissolved in DMF (4 mL) in a 5 mL microwave vial. NaH (0.039 g, 1.62 mmol) was added slowly and the mixture was stirred at rt for 30 min. Chloro-N,N-dimethylacetamide (0.147 g, 1.21 mmol) was added and the reaction mixture was heated for 2.5 h at 130° C. in a microwave oven. The reaction mixture was evaporated in vacuo and the residue was redissolved in a mixture of DCM and water. The phases were separated and the aqueous phase was extracted with DCM (2×25 mL). The combined organic extracts were evaporated, redissolved in MeOH and purified by preparative HPLC Method B. This afforded an oil which was treated with HCl in diethyl ether to give a solid material. Recrystallization from acetone and MeOH afforded 75 mg (41%) of the title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08846677B2 |
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| Quelldatensatz | uspto-grants-2014_09 |
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| ORD ID | ord-e49e647437524d0ebcef3596546110ac |
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| Quellennotiz | uspto-grants-2014_09 |
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