HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanesulfonic acid → n-{2-Tert-butyl-1-[(4,4-difluorocyclohexyl)methyl]-1h-benzimidazol-5-yl}ethanesulfonamide esylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanesulfonic acid | HCID 11668 | — |
| Reactant | Ethanesulfonamide, N-(1-((4,4-difluorocyclohexyl)methyl)-2-(1,1-dimethylethyl)-1H-benzimidazol-5-yl)- | HCID 11675994 | — |
| Solvent | tert-Butyl methyl ether | HCID 15413 | — |
| Product | n-{2-Tert-butyl-1-[(4,4-difluorocyclohexyl)methyl]-1h-benzimidazol-5-yl}ethanesulfonamide esylate | HCID 16742587 | 75% |
Reaction Steps
N-{2-tert-butyl-1-[(4,4-difluorocyclohexyl)methyl]-1H-benzimidazol-5-yl}ethanesulfonamide (111 mg) was slurried in methyl tert-butyl ether (2.1 ml) at 48° C. and ethane sulphonic acid (23 μl, 95%) was added. Shortly after the slurry became thinner and then recrystallised into a thicker slurry which was left over night at room temperature. The resulting crystals were filtered off, washed with methyl tert-butyl ether (2×400 μl) and dried at 40° C. under vacuum. A total of 105 mg (yield 75%) crystalline N-{2-tert-butyl-1-[(4,4-difluorocyclohexyl)methyl]-1H-benzimidazol-5-yl}ethanesulfonamide esylate was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07566788B2 |
| Source dataset | uspto-grants-2009_07 |
| ORD ID | ord-240d4f8e088747f9be62236267c2a75b |
| Source note | uspto-grants-2009_07 |