Methanesulfonic Acid → ethyl 3-[[2-[[4-[(Z)-N'-hexoxycarbonylcarbamimidoyl]anilino]methyl]-1-methylbenzimidazole-5-carbonyl]-pyridin-2-ylamino]propanoate;methanesulfonic acid

HRID 1470525ノート

反応式

HRID 1470525 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]([CH2:40][CH2:41][C:42]([O:44][CH2:45][CH3:46])=[O:43])[C:8]([C:10]1[CH:39]=[CH:38][C:13]2[N:14]([CH3:37])[C:15]([CH2:17][NH:18][C:19]3[CH:24]=[CH:23][C:22]([C:25](=[NH:36])[NH:26][C:27]([O:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35])=[O:28])=[CH:21][CH:20]=3)=[N:16][C:12]=2[CH:11]=1)=[O:9].[CH3:47][S:48]([OH:51])(=[O:50])=[O:49]>CC(C)=O>[CH3:35][CH2:34][CH2:33][CH2:32][CH2:31][CH2:30][O:29][C:27](/[N:26]=[C:25](\[NH2:36])/[C:22]1[CH:21]=[CH:20][C:19]([NH:18][CH2:17][C:15]2[N:14]([CH3:37])[C:13]3[CH:38]=[CH:39][C:10]([C:8]([N:7]([C:2]4[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=4)[CH2:40][CH2:41][C:42]([O:44][CH2:45][CH3:46])=[O:43])=[O:9])=[CH:11][C:12]=3[N:16]=2)=[CH:24][CH:23]=1)=[O:28].[CH3:47][S:48]([OH:51])(=[O:50])=[O:49]

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 135565674Dabigatran Etexilate

生成物 1

HCID 11434065ethyl 3-[[2-[[4-[(Z)-N'-hexoxycarbonylcarbamimidoyl]anilino]methyl]-1-methylbenzimidazole-5-carbonyl]-pyridin-2-ylamino]propanoate;methanesulfonic acid

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

反応条件

温度
20 °C

実験手順

100 g of 1-methyl-2-[N-[4-(N-n-hexyloxycarbonylamidino)phenyl]amino methyl]benzimidazol-5-yl-carboxylicacid-N-(2-pyridyl)-N-(2-ethoxycarbonylethyl) amide was dissolved in 890 ml of acetone under heating. A solution of 15 g of methane sulfonic acid in 200 ml of acetone was added to the reaction mixture. The solution is filtered and after the addition of 77 ml of acetone cooled to approximately 20° C. The precipitated product was filtered and washed with acetone then dried at 50° C. under reduced pressure.

後処理

  1. temperatureunder heating
  2. filtrationThe solution is filtered
  3. additionafter the addition of 77 ml of acetone
  4. filtrationThe precipitated product was filtered
  5. washwashed with acetone
  6. customthen dried at 50° C. under reduced pressure

出典と根拠

ORDレコード
ord-00932948f0fe4086aff20bd266b58d45
出典データセット
uspto-grants-2015_04
特許番号
US09006448B2

反応ノート

読み込み中…