HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Allyl chloroformate → Allyl-3-methanesulphonyloxy-pyrrolidine-1-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Allyl chloroformate | HCID 18052 | — |
| Edukt | (S)-1-Benzyl-3-mesyloxypyrrolidine | HCID 10934081 | — |
| Edukt | Methanol--water (1/1) | HCID 22242641 | — |
| Lösungsmittel | Heptane | HCID 8900 | — |
| Produkt | Allyl-3-methanesulphonyloxy-pyrrolidine-1-carboxylate | HCID 21832213 | — |
Reaktionsschritte
6.4 ml of allyl chloroformate were added dropwise to 10.2 g of methanesulphonic acid (S)-1-benzyl-pyrrolidin-3-yl ester in 880 ml of n-heptane at room temperature within 10 minutes under argon and with slight cooling. The two-phase mixture was stirred vigorously for 2 hours 45 minutes and subsequently treated with 40 ml of methanol/water (1:1). The aqueous methanolic phase was separated, extracted with 40 ml of heptane and thereafter the methanol was distilled off on a rotary evaporator. The aqueous phase was extracted twice with 30 ml of ethyl acetate. The organic phases were combined, dried over Na2SO4, filtered and the filtrate was concentrated. 8.23 g of beige oil were obtained.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05977381 |
| Quelldatensatz | uspto-grants-1999_11 |
| ORD ID | ord-3ae0e8dbf1aa4eb39309ecb2fee6b00a |
| Quellennotiz | uspto-grants-1999_11 |