HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 18401681, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4,6-Dichloropyrimidine | HCID 70943 | — |
| Reactant | Ethanamine, 2-(2-methoxyethoxy)-N,N-bis[2-(2-methoxyethoxy)ethyl]- | HCID 112414 | — |
| Reactant | 8-(3,5-Bis-trifluoromethyl-benzoyl)-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-one | HCID 18401725 | — |
| Catalyst | Cuprous chloride | HCID 62652 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 18401681 | HCID 18401681 | 24% |
Reaction Steps
A mixture of 8-(3,5-bis-trifluoromethyl-benzoyl)-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-one (0.1 g, 0.21 mmol), potassium carbonate (59 mg, 0.42 mmol), CuCl (2 mg, 0.021 mmol), tris[2-(2-methoxyethoxy)-ethyl]-amine (1.5 μL) and 4,6-dichloropyrimidine (32 mg, 0.21 mmol) in xylene (5 mL) was stirred and boiled for 18 h. The mixture was cooled, washed with water, ammonia in water (10%) and water again. Evaporation of the solvent yielded a residue which was purified by chromatography on silica gel (ethyl acetate/n-hexane 1:2) to yield the desired product (29 mg, 24%), m.p. 212-214° C. and MS: m/e=584.1 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06482829B2 |
| Source dataset | uspto-grants-2002_11 |
| ORD ID | ord-8618f2ce25ac4f02afc6fb00bf8c31c3 |
| Source note | uspto-grants-2002_11 |