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(C(C)=O)C(C)C.C(S(O)(=O)=O)C>C(C(C)=O)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
反応物 3
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 (210 mg) was dissolved in methyl iso-butyl ketone (2.1 ml). A solution was made of ethansulphonic acid (43.7 μl) and methyl iso-butyl ketone (1.0 ml). The methyl iso-butyl ketone/ethane sulphonic acid solution was added in a controlled manner over three hours. Thus, initially, to the base solution was added 2×20 μl acid solution. Then after 30 minutes three more additions were made (3×20 μl). Approximately 20 minutes later three additions of 40 μl acid solution was made and after 40 minutes 400 μl was added. Finally, 20 minutes later the remaining amount of acid solution was added. The resulting slurry was left 2.5 days with stirring before it was filtered off and washed with methyl iso-butyl ketone (2×200 μl). The product was dried at 40° C. under vacuum yielding 227 mg crystalline N-{2-tert-butyl-1-[(4,4-difluorocyclohexyl)methyl]-1H-benzimidazol-5-yl}ethanesulfonamide esylate salt. (yield 85%)
後処理
- addition400 μl was added
- additionFinally, 20 minutes later the remaining amount of acid solution was added
- waitThe resulting slurry was left 2.5 days
- filtrationwas filtered off
- washwashed with methyl iso-butyl ketone (2×200 μl)
- customThe product was dried at 40° C. under vacuum
出典と根拠
- ORDレコード
- ord-6a4f742e715f4a0d93e9f15a5c1ccd9c
- 出典データセット
- uspto-grants-2009_07
- 特許番号
- US07566788B2
関連ノート
読み込み中…