HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 19883248, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Iodoethane | HCID 6340 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 67900435 | HCID 67900435 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 19883248 | HCID 19883248 | 28% |
Reaction Steps
A mixture of 4-(4-chlorophenyl)-2-(4-trifluoromethylphenylamino) -5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine monohydrochloride (0.70 g, 1.73 mmol), triethylamine (0.5 mL, 3.6 mmol) and iodoethane (0.14 mL, 1.73 mmol) in ethanol (20 mL) was heated to reflux overnight. The mixture was cooled to room temperature, concentrated in vacuo, and chromatographed (silica gel, 5% methanol in methylene chloride). The hydrochloride salt was prepared by adding concentrated hydrochloric acid to a solution of the free base in methanol and recrystallized from acetone to give 0.21 g (28%) of 4-(4-chlorophenyl)-6-ethyl-2-(4-trifluromethylphenylamino)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine dihydrochloride monohydrate. m.p. 273°-275° C. MS: 433 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05137890 |
| Source dataset | uspto-grants-1992_08 |
| ORD ID | ord-03155931a3e54fa9b6c2d177a051e816 |
| Source note | uspto-grants-1992_08 |