HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethylcarbamoyl chloride → HCID 19799635, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethylcarbamoyl chloride | HCID 6916 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Calcium Chloride | HCID 5284359 | — |
| Reactant | HCID 19799580 | HCID 19799580 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 19799635 | HCID 19799635 | 60.1% |
Reaction Steps
A stirred slurry of 5 g (0.0163 mole) of 3-[3-(trifluoromethyl)phenoxy]azetidine oxalate in 50 ml of tetrahydrofuran was treated with 5 ml of triethylamine and after 1 hr, 2.5 g (0.018 mole) of diethylcarbamoyl chloride was added. After stirring an additional 15 hr, the reaction was treated with 10 ml of water and saturated with calcium chloride. The tetrahydrofruan was decanted from the solid residue and concentrated in vacuo to an oil. The crude oil was chromatographed on a Water's Prep-LC using 50% ethyl acetate/toluene as the eluent. After concentration of the main fractions 3.1 g (60.1%) of pale yellow oil was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05068231 |
| Source dataset | uspto-grants-1991_11 |
| ORD ID | ord-13c68b6100a949788e7eb142ba05e1f1 |
| Source note | uspto-grants-1991_11 |