HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethylamine → HCID 18924858, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethylamine | HCID 8021 | — |
| Reactant | HCID 18924851 | HCID 18924851 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 18924858 | HCID 18924858 | 44% |
Reaction Steps
A mixture of 2-chloromethyl-4-(3,4-dimethoxyphenyl)-5,6-dimethylthieno[2,3-d]pyrimidine (1.0 g), diethylamine (1.2 ml) and dichloromethane (30 ml) was stirred for 16 hours under reflux. The reaction mixture was concentrated under reduced pressure, which was dissolved in ethyl acetate. The ethyl acetate layer was washed with water and dried (MgSO4), then the solvent was distilled off. The residue was subjected to column chromatography on silica gel. From the fraction eluted with ethyl acetate-methanol (5:1, v/v), was obtained 4-(3,4-dimethoxyphenyl)-5,6-dimethyl-2-(N,N-dimethylamino-methyl)thieno[2,3-d]pyrimidine (0.49 g, 44%). Recrystallization from isopropyl ether gave colorless prisms, m.p.118°-120° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05747486 |
| Source dataset | uspto-grants-1998_05 |
| ORD ID | ord-dd322dead33a4bf28942748923428705 |
| Source note | uspto-grants-1998_05 |