HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 3-(4,6-Dimethoxypyrimidine-2-yl)-2-methylindole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phenylhydrazine | HCID 7516 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 1-(4,6-Dimethoxypyrimidin-2-yl)propan-2-one | HCID 11264052 | — |
| Catalyst | Zincchloride | HCID 3007855 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 3-(4,6-Dimethoxypyrimidine-2-yl)-2-methylindole | HCID 12979368 | 62% |
Reaction Steps
In 10 ml of toluene were dissolved 1.61 g (8.2 m moles) of 1-(4,6-dimethoxypyrimidine-2-yl)-2-propanone and 1.08 g (10 m moles) of phenylhydrazine. Thereto was added 1.36 g (10 m moles) of zinc chloride, followed by refluxing for 1 hour. The reaction mixture was allowed to cool, and ethyl acetate and water were added to dissolve the whole reaction mixture. The oily layer was washed with water, separated and dried over Glauber's salt. The resulting oily layer was concentrated under reduced pressure to obtain an orange solid. The solid was recrystallized from methanol to obtain 1.37 g (5.1 m moles) of 3-(4,6-dimethoxypyrimidine-2-yl)-2-methylindole. Yield: 62% Melting point: 182 to 184° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07504503B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-38b8c05896324093813bf0b9a1a53a4f |
| Source note | uspto-grants-2009_03 |