Doxazosin → Doxazosin Mesylate

HRID 1016363

反応式

HRID 1016363 の反応式
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH3:6][O:7][C:8]1[CH:9]=[C:10]2[C:19]([NH2:20])=[N:18][C:17]([N:21]3[CH2:26][CH2:25][N:24]([C:27]([CH:29]4[O:38][C:37]5[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=5[O:31][CH2:30]4)=[O:28])[CH2:23][CH2:22]3)=[N:16][C:11]2=[CH:12][C:13]=1[O:14][CH3:15].CN1CCCC1=O>CO>[CH3:6][O:7][C:8]1[CH:9]=[C:10]2[C:19]([NH2:20])=[N:18][C:17]([N:21]3[CH2:22][CH2:23][N:24]([C:27]([CH:29]4[O:38][C:37]5[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=5[O:31][CH2:30]4)=[O:28])[CH2:25][CH2:26]3)=[N:16][C:11]2=[CH:12][C:13]=1[O:14][CH3:15].[CH3:1][S:2]([OH:5])(=[O:4])=[O:3]

参加物

5

反応物 3

HCID 3157DoxazosinHCID 6395Methanesulfonic Acid2 回HCID 13387N-methyl-2-pyrrolidone

生成物 1

HCID 62978Doxazosin Mesylate収率 163.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

14.1 g of anhydrous methanesulfonic acid were added to a stirred mixture of 63.2 g of doxazosin, 125 ml of N-methyl-2-pyrrolidone and 500 ml of methanol in a 1 1 three-necked round-bottomed flask. During this time the internal temperature rose to 30° C., and a solution formed. After the addition of the methanesulfonic acid was complete, the reaction mixture was filtered into a second 1 1 three-necked round-bottomed flask. The filter was washed with 85 ml of methanol, and the combined filtrates were stirred for 5 h. After completion of the stirring time, the resulting precipitate was filtered off with suction and washed 3× with 25 ml of methanol each time. 125 g of moist doxazosin mesylate (modification D) were obtained. This corresponds to 70.4 g of dry substance and a yield of 91.8%.

後処理

  1. customrose to 30° C.
  2. customa solution formed
  3. filtrationthe reaction mixture was filtered into a second 1 1 three-necked round-bottomed flask
  4. washThe filter was washed with 85 ml of methanol
  5. filtrationAfter completion of the stirring time, the resulting precipitate was filtered off with suction
  6. washwashed 3× with 25 ml of methanol each time

出典と根拠

ORDレコード
ord-4efc50acdf4f4936b08c97e91de74653
出典データセット
uspto-grants-2002_11
特許番号
US06476033B1

関連ノート

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