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

HRID 1470525노트

반응식

HRID 1470525 반응식
[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]

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 135565674Dabigatran Etexilate

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매2회

반응 조건

온도
20 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-00932948f0fe4086aff20bd266b58d45
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09006448B2

반응 노트

불러오는 중…