HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → 2-Chloro-9-cyclobutyl-7,7-difluoro-5-methyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 2-Chloro-9-cyclobutyl-7,7-difluoro-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one | HCID 86637502 | — |
| Solvent | Water | HCID 962 | — |
| Product | 2-Chloro-9-cyclobutyl-7,7-difluoro-5-methyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one | HCID 86637503 | — |
Reaction Steps
To a mixture of 5.5 g (0.0191 mole) of 2-chloro-9-cyclobutyl-7,7-difluoro-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (VI-1), 25 mL of dimethylformamide and 9.4 g (0.0287 mole) of cesium carbonate was added 10.9 g (0.0764 mole) of iodomethane. The mixture was stirred for 3 hours, then 80 mL of water was added and the solid collected by suction filtration to give 4.8 g of 2-chloro-9-cyclobutyl-7,7-difluoro-5-methyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (VII-1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08003785B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-e5c953a508954cd1bb59a66097cacd56 |
| Source note | uspto-grants-2011_08 |