HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → HCID 10025688, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Chlorotrimethylsilane | HCID 6397 | — |
| Reactant | HCID 10025689 | HCID 10025689 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Methyl Ethyl Ketone | HCID 6569 | — |
| Product | HCID 10025688 | HCID 10025688 | — |
Reaction Steps
In the manner described for Example 27, 255 mg of the polar diastereoisomer of 1-(4-dimethylamino-4-phenylcyclohexylmethyl)-3-(3-phenylpropyl)urea were also obtained (m.p. 159–165° C.). 249 mg (0.63 mmol.) thereof were dissolved in acetone (7 ml) and 2-butanone (15 ml), and chlorotrimethylsilane (121 μl, 0.95 mmol.) was added dropwise at RT, with stirring. After stirring for 1 h, the reaction solution was reduced to about 0.5 ml in vacuo, ether (10 ml) was added thereto, and vigorous stirring was carried out for 1 h at RT. The resulting solid was filtered off with suction, washed with ether (3×2.5 ml) and dried in vacuo. 270 mg of the corresponding hydrochloride of the polar urea were obtained (greyish-white solid, m.p. 100–110° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07173045B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-8adfefd98944466eaddaf8dbdb2b416d |
| Source note | uspto-grants-2007_02 |