HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 178512366, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Cyanamide | HCID 9864 | — |
| Reactant | HCID 178504028 | HCID 178504028 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178512366 | HCID 178512366 | 77.1% |
Reaction Steps
450 mg of N-(10H-pyrazino[2,3-b][1,4]benzothiazin-8-ylmethyl)-S-methylisothiourea and 500 mg of cyanamide were heated in 30 ml of N,N-dimethylformamide to 70° C. for 12 hours. Then the reaction mixture was brought back to room temperature and distributed into water and ethyl acetate. The organic layer was extracted and washed with water. After adding 5 g of silica gel, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol/aqueous ammonia) to thereby give 340 mg of the title compound as yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06518423B1 |
| Source dataset | uspto-grants-2003_02 |
| ORD ID | ord-c985b0f7246b43c580c8bfeafc85446c |
| Source note | uspto-grants-2003_02 |