Ethanesulfonic acid → n-{2-Tert-butyl-1-[(4,4-difluorocyclohexyl)methyl]-1h-benzimidazol-5-yl}ethanesulfonamide esylate

HRID 230716

반응식

HRID 230716 반응식
[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(=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]

참가 물질

4

반응물 2

HCID 11668Ethanesulfonic acidHCID 11675994Ethanesulfonamide, N-(1-((4,4-difluorocyclohexyl)methyl)-2-(1,1-dimethylethyl)-1H-benzimidazol-5-yl)-

생성물 1

HCID 16742587n-{2-Tert-butyl-1-[(4,4-difluorocyclohexyl)methyl]-1h-benzimidazol-5-yl}ethanesulfonamide esylate

시약·촉매·용매 1

HCID 7915Isopropyl Acetate용매

실험 절차

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.

후처리

  1. customCrystallisation
  2. filtrationwas filtered off
  3. washwashed with iso-propylacetate (3×200 μl)
  4. customThe product was dried at 40° C. under vacuum

출처 및 근거

ORD 기록
ord-63b34ebc74ce45e1b1f7475b5d285e03
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07566788B2

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