HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 12093240, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 66753597 | HCID 66753597 | — |
| Reactant | HCID 68601695 | HCID 68601695 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 12093240 | HCID 12093240 | — |
Reaction Steps
A mixture of 260 mg of 3-methyl-7-(3-methyl-2-buten-1-yl)-8-[3-(tert.-butyloxy-carbonylamino)-piperidin-1-yl]-xanthine, 185 mg of 4-bromo-methyl-1-methyl-1H-benzo[c][1,2]thiazine-2,2-dioxide and 550 mg of potassium carbonate in 4 ml N,N-dimethylformamide is stirred for about 40 h at ambient temperature. As no reaction of any note can be detected by thin layer chromatography, the mixture is heated to 60° C. for 2 h and then stirred for another 15 h at 50° C. until the reaction is virtually complete. Then 30 ml of water are added, the precipitate formed is suction filtered and dried. The crude product is purified by chromatography over a silica gel column with petroleum ether/ethyl acetate (1:1) as eluant.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07482337B2 |
| Source dataset | uspto-grants-2009_01 |
| ORD ID | ord-ab055c6bcf534916bdb577dbacfe543a |
| Source note | uspto-grants-2009_01 |