HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 3-[1-(4-Pyridinylmethyl)-2-pyrrolidinyl]phenyl methylcarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Methyl Isocyanate | HCID 12228 | — |
| Reactant | 3-[1-(4-Pyridinylmethyl)-2-pyrrolidinyl]phenol | HCID 15293226 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3-[1-(4-Pyridinylmethyl)-2-pyrrolidinyl]phenyl methylcarbamate | HCID 9904825 | 86% |
Reaction Steps
To a stirred solution of 3-[1-(4-pyridinylmethyl)-2-pyrrolidinyl]phenol (0.60 g) in dry tetrahydrofuran (16 ml) was added milled potassium carbonate (0.36 g), followed by methyl isocyanate (0.15 ml), dropwise, at ambient temperature, under nitrogen, with stirring. The mixture was stirred for 17 hrs and filtered through a pad of celite. The filter cake was washed with ethyl acetate, and the filtrate was concentrated. The residue was purified by flash column chromatography (silica gel, ether). The appropriate fractions were collected and concentrated to afford 0.63 g (86%) of product. Trituration of the residue with petroleum ether gave the analytical sample, mp 92°-105° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05591856 |
| Source dataset | uspto-grants-1997_01 |
| ORD ID | ord-03371d36ffa34441bb2f5e6cba92eb12 |
| Source note | uspto-grants-1997_01 |