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

HRID 323320
ノート
印刷プレビュー

反応式

HRID 323320 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:46]=[C:47]([O:51][CH3:52])[C:48]=1[O:49][CH3:50])[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][C:36]4[S:37][C:38]([Cl:41])=[CH:39][CH:40]=4)[C:33]4[CH:42]=[CH:43][CH:44]=[CH:45][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].[CH3:53][S:54]([OH:57])(=[O:56])=[O:55].C(OCC)(=O)C>CO>[CH3:53][S:54]([OH:57])(=[O:56])=[O:55].[CH3:52][O:51][C:47]1[CH:46]=[C:5]([CH:4]=[C:3]([O:2][CH3:1])[C:48]=1[O:49][CH3:50])[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][C:36]4[S:37][C:38]([Cl:41])=[CH:39][CH:40]=4)[C:33]4[CH:42]=[CH:43][CH:44]=[CH:45][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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6395Methanesulfonic AcidHCID 8857Ethyl AcetateHCID 98535341-(3,4,5-trimethoxybenzoyl)-3-(2-(4-(1-(5-chlorothien-2-ylmethyl)-1H-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-(3,4-difluorophenyl) Pyrrolidine

生成物 1

HCID 220092511-(3,4,5-Trimethoxybenzoyl)-3-(2-(4-(1-(5-chlorothien-2-ylmethyl)-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 887Methanol溶媒

実験手順

Combine 1-(3,4,5-trimethoxybenzoyl)-3-(2-(4-(1-(5-chlorothien-2-ylmethyl)-1H-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-(3,4-difluorophenyl) pyrrolidine (1.21 g, 1.61 mmol), and methanesulfonic acid (0.23 mL, 3.54 mmol), ethyl acetate (90 mL), and methanol (10 mL) and stir. After 18 hours, filter and evaporate the filtrate in vacuo to give a residue. Triturate the residue with diethyl ether to give a solid. Decant the solvent and add diethyl ether. Collect the solid by filtration and dry in vacuo at 82° C. to give the title compound. Elemental Analysis calculated for C39H42ClF2N5O4S.2 CH3SO3H.1.8 H2O: C, 50.52; H, 5.54; N, 7.18. Found: C, 50.67; H, 5.38; N, 7.22.

後処理

  1. filtrationfilter
  2. customevaporate the filtrate in vacuo
  3. customto give a residue
  4. customTriturate the residue with diethyl ether
  5. customto give a solid
  6. customDecant the solvent
  7. additionadd diethyl ether
  8. customCollect the solid
  9. filtrationby filtration
  10. customdry in vacuo at 82° C.

出典と根拠

ORDレコード
ord-613d6facb14b4056845072a6ef365cde
出典データセット
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06211199B1

反応ノート

読み込み中…

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