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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 | Isopropyl Acetate | HCID 7915 | — |
| 生成物 | n-{2-Tert-butyl-1-[(4,4-difluorocyclohexyl)methyl]-1h-benzimidazol-5-yl}ethanesulfonamide esylate | HCID 16742587 | — |
反応手順
N-{2-tert-butyl-1-[(4,4-difluorocyclohexyl)methyl]-1H-benzimidazol-5-yl}ethanesulfonamide (101 mg) was dissolved in iso-propylacetate (1.5 ml) at 42° C. and ethane sulphonic acid (20 μl, 95%) was added. Crystallisation started immediately. The slurry was left for three days before it was filtered off and washed with iso-propylacetate (3×200 μl). The product was dried at 40° C. under vacuum to yield 61 mg crystalline N-{2-tert-butyl-1-[(4,4-difluorocyclohexyl)methyl]-1H-benzimidazol-5-yl}ethanesulfonamide esylate salt.
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-63b34ebc74ce45e1b1f7475b5d285e03 |
| 出典メモ | uspto-grants-2009_07 |