Oxalic Acid → 1-methyl-2[N-[4-amidinophenyl]aminomethyl]benzimidazol-5-yl-carboxylicacid-N-(2-pyridyl)-N-(2-ethoxycarbonylethyl)amide oxalate

HRID 1470514

反応式

HRID 1470514 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]([CH2:31][CH2:32][C:33]([O:35][CH2:36][CH3:37])=[O:34])[C:8]([C:10]1[CH:30]=[CH:29][C:13]2[N:14]([CH3:28])[C:15]([CH2:17][NH:18][C:19]3[CH:24]=[CH:23][C:22]([C:25](=[NH:27])[NH2:26])=[CH:21][CH:20]=3)=[N:16][C:12]=2[CH:11]=1)=[O:9].[C:38]([OH:43])(=[O:42])[C:39]([OH:41])=[O:40]>C(O)C>[C:38]([OH:43])(=[O:42])[C:39]([OH:41])=[O:40].[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]([CH2:31][CH2:32][C:33]([O:35][CH2:36][CH3:37])=[O:34])[C:8]([C:10]1[CH:30]=[CH:29][C:13]2[N:14]([CH3:28])[C:15]([CH2:17][NH:18][C:19]3[CH:24]=[CH:23][C:22]([C:25](=[NH:26])[NH2:27])=[CH:21][CH:20]=3)=[N:16][C:12]=2[CH:11]=1)=[O:9]

参加物

4

反応物 2

HCID 971Oxalic AcidHCID 446804Dabigatran Ethyl Ester

生成物 1

HCID 573893471-methyl-2[N-[4-amidinophenyl]aminomethyl]benzimidazol-5-yl-carboxylicacid-N-(2-pyridyl)-N-(2-ethoxycarbonylethyl)amide oxalate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

反応条件

温度
55 °C

実験手順

A mixture of 1-methyl-2-[N-[4-amidinophenyl]aminomethyl]benzimidazol-5-yl-carboxylicacid-N-(2-pyridyl)-N-(2-ethoxycarbonylethyl)amide compound of formula-5 (100 g) and ethanol (1200 ml) was heated to 50-60° C. A solution of oxalic acid (25.25 g) in ethanol (1500 ml) was added to the above reaction mixture at 50-60° C. and stirred for 45 minutes. The reaction mixture was cooled to 25-35° C. and stirred for 6 hours at 25-35° C. Filtered the solid, washed with ethanol and then dried to get the title compound.

後処理

  1. temperatureThe reaction mixture was cooled to 25-35° C.
  2. stirringstirred for 6 hours at 25-35° C
  3. filtrationFiltered the solid
  4. washwashed with ethanol
  5. customdried

出典と根拠

ORDレコード
ord-d548663fb9c64f02b3ede67f1688ca4a
出典データセット
uspto-grants-2015_04
特許番号
US09006448B2

関連ノート

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