HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Isopropenyl chloroformate → (3S)-6-Chloro-1-(isopropenyloxycarbonyl)-3-methyl-3,4-dihydro-1,4,5-triazanaphthalen-2(1H)-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Isopropenyl chloroformate | HCID 93846 | — |
| Edukt | (3S)-6-Chloro-3-methyl-3,4-dihydro-1,4,5-triazanaphthalen-2(1H)-one | HCID 57066600 | — |
| Lösungsmittel | Pyridine | HCID 1049 | — |
| Produkt | (3S)-6-Chloro-1-(isopropenyloxycarbonyl)-3-methyl-3,4-dihydro-1,4,5-triazanaphthalen-2(1H)-one | HCID 57158666 | — |
Reaktionsschritte
The compound of Example 2 (988 mg, 5.0 mmol) was dissolved in 30 ml of anhydrous pyridine. After addition of 0.6 ml (5.5 mmol) of isopropenyl chloroformate, the mixture was stirred at room temperature for 4 h and subsequently concentrated. The residue was dissolved in ethyl acetate and washed three times with water, dried (sodium sulfate) and concentrated. After chromatography on silica gel (ethyl acetate/heptane=1:2), the desired compound was isolated and crystallized from diethyl ether/pentane; yield 380 mg (27%) of melting point 86°-87° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05424311 |
| Quelldatensatz | uspto-grants-1995_06 |
| ORD ID | ord-6d6ed009073d40378300b3f99b4e6525 |
| Quellennotiz | uspto-grants-1995_06 |