HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → HCID 58424601, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | Thiourea | HCID 2723790 | — |
| Reactant | HCID 67173773 | HCID 67173773 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 58424601 | HCID 58424601 | — |
Reaction Steps
The above mixture of 2-(6-bromo-2-phenylchroman-4-ylidene)ethyl carbamimidothioate HCl salt and thiourea is dissolved in TFA (4 mL) containing MeSO3H (0.4 mL) and stirred at rt for 1 h. The solvent is removed under reduced pressure. The residue is dissolved in ethyl acetate and washed with sat NaHCO3. The separated aqueous phase is extracted with ethyl acetate once and the combined organic phases are washed with brine, and dried over Na2SO4, and filtered. The filtrate is concentrated to give crude 6-bromo-2-phenyl-5′,6′-dihydrospiro[chroman-4,4′-[1,3]thiazin]-2′-amine, which is used for next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08921359B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-7595e3b4c18045b8b57fa6b0989a4e5c |
| Source note | uspto-grants-2014_12 |