Doxazosin → Doxazosin Mesylate

HRID 2301285

反応式

HRID 2301285 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]>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

4

反応物 2

HCID 3157DoxazosinHCID 6395Methanesulfonic Acid2 回

生成物 1

HCID 62978Doxazosin Mesylate収率 148%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

17.7 g of anhydrous methanesulfonic acid were added to a stirred mixture of 79.0 g of doxazosin and 800 ml of methanol in a 2 l three-neck round-bottom flask. The internal temperature rose to 30° C. during this, and a solution was produced. After the addition of methanesulfonic acid was complete, the mixture was stirred for 5 h. The resulting precipitate was then.filtered off with suction and washed 3× with 50 ml of methanol each time. 141.8 g of moist doxazosin mesylate (modification D) were obtained. This corresponds to 89.2 g of dry substance and a yield of 93.1%.

後処理

  1. customrose to 30° C.
  2. customwas produced
  3. washwashed 3× with 50 ml of methanol each time

出典と根拠

ORDレコード
ord-71ec313975fa4d0d884030b6bb662395
出典データセット
uspto-grants-2002_12
特許番号
US06500830B1

関連ノート

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