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Ethanesulfonic acid → n-{2-Tert-butyl-1-[(4,4-difluorocyclohexyl)methyl]-1h-benzimidazol-5-yl}ethanesulfonamide esylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanesulfonic acid | HCID 11668 | — |
| 反応物 | Ethanesulfonamide, N-(1-((4,4-difluorocyclohexyl)methyl)-2-(1,1-dimethylethyl)-1H-benzimidazol-5-yl)- | HCID 11675994 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | n-{2-Tert-butyl-1-[(4,4-difluorocyclohexyl)methyl]-1h-benzimidazol-5-yl}ethanesulfonamide esylate | HCID 16742587 | 75% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07566788B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-240d4f8e088747f9be62236267c2a75b |
| 出典メモ | uspto-grants-2009_07 |