HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorosulfamic acid → HCID 23155691, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorosulfamic acid | HCID 24499 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 23155641 | HCID 23155641 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 23155691 | HCID 23155691 | 75% |
Reaction Steps
In 3 ml of N-methylpyrrolidone, 105 mg of 7-hydroxy-1-octahydropyrido[1,2-a]pyrazin-2-ylisoquinoline as synthesized in Production Example 84 was dissolved, and to the solution 1.00 g of sulfamoyl chloride was added, followed by an hour's stirring at room temperature. The solution was neutralized with saturated aqueous sodium hydrogencarbonate solution, extracted with chloroform, dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified on silica gel column chromatography (25% aqueous ammonia:methanol:chloroform=1:10:90) to provide 85 mg (75%) of 1-octahydropyrido[1,2-a]pyrazin-2-yl-7-sulfamoylisoquinoline.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07799775B2 |
| Source dataset | uspto-grants-2010_09 |
| ORD ID | ord-82bca172f51e425f95d7354f4cbed2d7 |
| Source note | uspto-grants-2010_09 |