HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorosulfonic acid → HCID 90419007, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorosulfonic acid | HCID 24638 | — |
| Reactant | 6-Chloro-N-methyl-1,3-benzothiazol-2-amine | HCID 10774358 | — |
| Product | HCID 90419007 | HCID 90419007 | — |
Reaction Steps
A solution of 6-chloro-N-methylbenzo[d]thiazol-2-amine (500 mg, 2.53 mmol) in chlorosulfonic acid (5 mL) was stirred at 130° C. overnight. The solution was allowed to cool and slowly added to a large excess of ice. The aqueous layer was extracted with EtOAc (3×50 mL). The combined organic layers were washed with brine, dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by chorography (silica gel) eluting with PE/EA=1:1 to get the title compound. 1H NMR (CHLOROFORM-d) δ: 7.95 (d, J=1.9 Hz, 1H), 7.89 (d, J=2.1 Hz, 1H), 6.70 (br. s., 1H), 3.16 (d, J=4.3 Hz, 3H). LC-MS: m/z 297 (M+H)+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09108921B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-6dda2be8c55e4ec8b146747b4cb9e337 |
| Source note | uspto-grants-2015_08 |