Methanesulfonic Acid → 1-(3,4,5-Trimethoxybenzoyl)-3-(2-(4-(1-(2-methylsulfonylethyl)-1h-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-(3,4-difluorophenyl) pyrrolidine methanesulfonic acid salt

HRID 323327노트

반응식

HRID 323327 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:45]=[C:46]([O:50][CH3:51])[C:47]=1[O:48][CH3:49])[C:6]([N:8]1[CH2:12][CH2:11][C:10]([CH2:21][CH2:22][N:23]2[CH2:28][CH2:27][CH:26]([NH:29][C:30]3[N:34]([CH2:35][CH2:36][S:37]([CH3:40])(=[O:39])=[O:38])[C:33]4[CH:41]=[CH:42][CH:43]=[CH:44][C:32]=4[N:31]=3)[CH2:25][CH2:24]2)([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[C:15]([F:20])[CH:14]=2)[CH2:9]1)=[O:7].C(OCC)(=O)C.[CH3:58][S:59]([OH:62])(=[O:61])=[O:60]>C(OCC)C>[CH3:58][S:59]([OH:62])(=[O:61])=[O:60].[CH3:51][O:50][C:46]1[CH:45]=[C:5]([CH:4]=[C:3]([O:2][CH3:1])[C:47]=1[O:48][CH3:49])[C:6]([N:8]1[CH2:12][CH2:11][C:10]([CH2:21][CH2:22][N:23]2[CH2:28][CH2:27][CH:26]([NH:29][C:30]3[N:34]([CH2:35][CH2:36][S:37]([CH3:40])(=[O:38])=[O:39])[C:33]4[CH:41]=[CH:42][CH:43]=[CH:44][C:32]=4[N:31]=3)[CH2:25][CH2:24]2)([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[C:15]([F:20])[CH:14]=2)[CH2:9]1)=[O:7]

참가 물질

5

반응물 3

HCID 6395Methanesulfonic AcidHCID 8857Ethyl AcetateHCID 9853348HCID 9853348, 화합물

생성물 1

HCID 220091761-(3,4,5-Trimethoxybenzoyl)-3-(2-(4-(1-(2-methylsulfonylethyl)-1h-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-(3,4-difluorophenyl) pyrrolidine methanesulfonic acid salt

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

Combine 1-(3,4,5-trimethoxybenzoyl)-3-(2-(4-(1-(2-methylsulfonylethyl)-1H-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-(3,4-difluorophenyl) pyrrolidine (1.0 g, 1.38 mmol) and ethyl acetate (50 mL). Add methanesulfonic acid (0.27 g, 2.76 mmol). Heat to reflux. After 1 hour, cool to ambient temperature and stir. After 40 hours, add diethyl ether (150 mL) to give a solid. Repeatedly, decant the solvent add diethyl ether before collecting the solid and drying in vacuo to give the title compound.

후처리

  1. temperatureHeat to reflux
  2. waitAfter 40 hours
  3. customto give a solid
  4. customRepeatedly, decant the solvent
  5. additionadd diethyl ether
  6. custombefore collecting the solid
  7. customdrying in vacuo

출처 및 근거

ORD 기록
ord-a474e043dcc4479ab42d4422e919f057
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211199B1

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