Methanesulfonic Acid → Eprosartan Mesylate

HRID 1808665ノート

反応式

HRID 1808665 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収率 74.4%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
8 °C

実験手順

Crude eprosartan free base (50 gm, obtained in reference example 1) is stirred with isopropyl alcohol (750 ml), the reaction mass is cooled to 8° C. and then methane sulfonic acid (34 gm) is added drop wise to the mass at 0-5° C. The reaction mass is stirred for 5 hours 30 minutes at 0-5° C., the mass filtered, the material washed with isopropyl alcohol (138 ml) and then dried under vacuum at 45° C. to give 45.6 gm of crude eprosartan mesylate (HPLC purity: 98.7%).

後処理

  1. filtrationthe mass filtered
  2. washthe material washed with isopropyl alcohol (138 ml)
  3. customdried under vacuum at 45° C.

出典と根拠

ORDレコード
ord-e0d4db903aca4cb494c01305162df421
出典データセット
uspto-grants-2013_01
特許番号
US08361507B2

反応ノート

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