HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid monohydrate → 2-Bromo-5-methyl-4,5,6,7-tetrahydrothiazolo[5,4-c]pyridine 4-methylbenzenesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | 2-Bromo-5-methyl-4,5,6,7-tetrahydrothiazolo(5,4-c)pyridine | HCID 11172335 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 2-Bromo-5-methyl-4,5,6,7-tetrahydrothiazolo[5,4-c]pyridine 4-methylbenzenesulfonate | HCID 11211875 | 87.9% |
Reaction Steps
2-Bromo-5-methyl-4,5,6,7-tetrahydrothiazolo[5,4-c]pyridine (557.6 g) was dissolved in methanol (3.9 L), and to the solution was added dropwise a solution of p-toluenesulfonic acid monohydrate (500.0 g) in methanol (1.7 L) at 30° C. The resultant mixture was stirred at the same temperature for 1 hour, and then at or below 10° C. for 2 hours. The precipitated crystals were collected by filtration, and were washed with methanol (1.1 L), followed by drying at 40° C. under reduced pressure, to thereby give 851.9 g of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08058440B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-f97d4e12307341469aaa0f9a8f8342b5 |
| Source note | uspto-grants-2011_11 |