HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 3-[1-Ethyl-2-pyrrolidinyl]phenyl methylcarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Methyl Isocyanate | HCID 12228 | — |
| Reactant | 3-[1-Ethyl-2-pyrrolidinyl]phenol | HCID 23361312 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3-[1-Ethyl-2-pyrrolidinyl]phenyl methylcarbamate | HCID 15222798 | 96% |
Reaction Steps
To a solution of 3-[1-ethyl-2-pyrrolidinyl]phenol (0.8 g) in dry tetrahydrofuran (40 ml) was added methyl isocyanate (0.26 ml) at ambient temperature, under nitrogen, with stirring for ten mins. Milled potassium carbonate was added and the reaction mixture was stirred for 4 hrs, and filtered through a pad of celite. The solids were washed with ethyl acetate, and the combined filtrates were concentrated. The residue was purified by flash column chromatography (silica gel, dichloromethane/0-30% methanol), and the eluant flushed through alumina (ethyl acetate) to give 1.0 g (96%) of product. Recrystallization from ether/petroleum ether gave the analytical sample, mp 67°-69° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05554750 |
| Source dataset | uspto-grants-1996_09 |
| ORD ID | ord-c0134649fdfc47868317a08c8f24e7b7 |
| Source note | uspto-grants-1996_09 |