Methanesulfonic Acid → Eprosartan Mesylate

HRID 1808667

反応式

HRID 1808667 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.C([O-])(=O)C.[CH3:35][S:36]([OH:39])(=[O:38])=[O:37]>CC(C)=O>[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.[CH3:35][S:36]([OH:39])(=[O:38])=[O:37]

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 86643031HCID 86643031、化合物

生成物 1

HCID 5282474Eprosartan Mesylate収率 89.8%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
2.5 °C

実験手順

Eprosartan acetate (30 gm, obtained in example 1) is suspended in acetone (450 ml) at 25-30° C., the suspension is cooled to 0-5° C., methanesulfonic acid (21.2 gm) is added drop wise while maintaining the temperature at 0-5° C. The temperature of the mass is raised to 25-30° C. and stirred for 5 hours. The mass is cooled to 0-5° C., stirred for 1 hour, the material is filtered and then suck dried. To the resulting wet cake is added acetone (60 ml) and stirred for 30 minutes at 25-30° C. The material is filtered, washed with acetone (30 ml) and then dried to give 29 gm of pure eprosartan mesylate [HPLC Purity: 99.95%; Specific Surface Area: 1.09 m2/g; Mean particle size (D50): 12.13 μm and 90 volume-% of the particles (D90): 33.48 μm].

後処理

  1. temperaturewhile maintaining the temperature at 0-5° C
  2. temperatureThe temperature of the mass is raised to 25-30° C.
  3. temperatureThe mass is cooled to 0-5° C.
  4. stirringstirred for 1 hour
  5. filtrationthe material is filtered
  6. customsuck dried
  7. additionTo the resulting wet cake is added acetone (60 ml)
  8. stirringstirred for 30 minutes at 25-30° C
  9. filtrationThe material is filtered
  10. washwashed with acetone (30 ml)
  11. customdried

出典と根拠

ORDレコード
ord-35f8ef45cea9444dac6cf8153a70d751
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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