Methanesulfonic Acid → Eprosartan Mesylate

HRID 1808663

反応式

HRID 1808663 の反応式
[CH3:1][CH2:2][CH2:3][CH2:4][C:5]1[N:9]([CH2:10][C:11]2[CH:12]=[CH:13][C:14]([C:17]([OH:19])=[O:18])=[CH:15][CH:16]=2)[C:8](/[CH:20]=[C:21](/[C:28]([OH:30])=[O:29])\[CH2:22][C:23]2[S:27][CH:26]=[CH:25][CH:24]=2)=[CH:7][N:6]=1.[CH3:31][S:32]([OH:35])(=[O:34])=[O:33]>C(O)(C)C>[CH3:1][CH2:2][CH2:3][CH2:4][C:5]1[N:9]([CH2:10][C:11]2[CH:12]=[CH:13][C:14]([C:17]([OH:19])=[O:18])=[CH:15][CH:16]=2)[C:8](/[CH:20]=[C:21](/[C:28]([OH:30])=[O:29])\[CH2:22][C:23]2[S:27][CH:26]=[CH:25][CH:24]=2)=[CH:7][N:6]=1.[CH3:31][S:32]([OH:35])(=[O:34])=[O:33]

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 5281037Eprosartan

生成物 1

HCID 5282474Eprosartan Mesylate

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
8 °C

実験手順

As per the process described and exemplified in the U.S. Pat. No. 5,185,351 (herein after referred to as the '351 patent), eprosartan free base (obtained as per the processes described in example I of the '351 patent) is suspended in isopropyl alcohol under stirring at about 8° C., methanesulfonic acid is added rapidly to the stirred suspension, the mass cooled to 3° C. and the precipitated solid collected to give crude eprosartan mesylate. The crude eprosartan mesylate is further purified by dissolving crude eprosartan mesylate in acetic acid at 80° C., filtered through a hyflow bed at 80° C., the solution cooled slowly to 25° C. followed by stirring and then the precipitated solid is collected by adding ethyl acetate as an anti-solvent to give eprosartan mesylate.

後処理

  1. customobtained as per the processes
  2. temperaturethe mass cooled to 3° C.
  3. customthe precipitated solid collected
  4. customto give crude eprosartan mesylate
  5. customThe crude eprosartan mesylate is further purified
  6. dissolutionby dissolving crude eprosartan mesylate in acetic acid at 80° C.
  7. filtrationfiltered through a hyflow bed at 80° C.
  8. temperaturethe solution cooled slowly to 25° C.
  9. stirringby stirring
  10. customthe precipitated solid is collected
  11. additionby adding ethyl acetate as an anti-solvent

出典と根拠

ORDレコード
ord-aaf8478e97c44019b00c510f86452a37
出典データセット
uspto-grants-2013_01
特許番号
US08361507B2

関連ノート

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