反応式
[C:1]([C:5]1[N:9]([CH2:10][CH:11]2[CH2:16][CH2:15][C:14]([F:18])([F:17])[CH2:13][CH2:12]2)[C:8]2[CH:19]=[CH:20][C:21]([NH:23][S:24]([CH2:27][CH3:28])(=[O:26])=[O:25])=[CH:22][C:7]=2[N:6]=1)([CH3:4])([CH3:3])[CH3:2].[CH2:29]([S:31]([OH:34])(=[O:33])=[O:32])[CH3:30]>C(OC)(C)(C)C>[S:31]([CH2:29][CH3:30])([OH:34])(=[O:33])=[O:32].[C:1]([C:5]1[N:9]([CH2:10][CH:11]2[CH2:12][CH2:13][C:14]([F:18])([F:17])[CH2:15][CH2:16]2)[C:8]2[CH:19]=[CH:20][C:21]([NH:23][S:24]([CH2:27][CH3:28])(=[O:25])=[O:26])=[CH:22][C:7]=2[N:6]=1)([CH3:4])([CH3:2])[CH3:3]参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
実験手順
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.
後処理
- customrecrystallised into a thicker slurry which
- waitwas left over night at room temperature
- filtrationThe resulting crystals were filtered off
- washwashed with methyl tert-butyl ether (2×400 μl)
- customdried at 40° C. under vacuum
出典と根拠
- ORDレコード
- ord-240d4f8e088747f9be62236267c2a75b
- 出典データセット
- uspto-grants-2009_07
- 特許番号
- US07566788B2
関連ノート
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