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 323327ノート

反応式

HRID 323327 の反応式
[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]

参加物

5

反応物 3

HCID 6395Methanesulfonic AcidHCID 8857Ethyl AcetateHCID 9853348HCID 9853348、化合物

生成物 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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a474e043dcc4479ab42d4422e919f057
出典データセット
uspto-grants-2001_04
特許番号
US06211199B1

反応ノート

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