Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | HCID 21487723 | HCID 21487723 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 178517451 | HCID 178517451 | — |
Reaction Steps
To a solution of 2.11 g of 2-trichloroacetamido-3-(o-fluorobenzoyl)thiophene in 18 ml of dimethylsulfoxide was added 0.89 g of ammonium acetate. The mixture was heated at 95° C for 2 hours and poured into ice water, and extracted with dichloromethane. The dichloromethane layer was washed with water, dried over sodium sulfate and the solvent was removed under reduced pressure. The residue was chromatographed on 60 g of Silica gel, using ethyl acetate as an eluent to obtain 4-(o-fluorophenyl)-1,2-dihydrothieno(2,3-d)-pyrimidin-2-one as crystals having a melting point of 272°-275° C. Recrystallization from acetone gave crystals melting at 247.5°- 249° C. The following compounds were prepared similarly:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04001412 |
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| Source dataset | uspto-grants-1977_01 |
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| ORD ID | ord-8bae8b5c4fe74aa6bdcd2f729d5f7d62 |
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| Source note | uspto-grants-1977_01 |
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