Doxazosin → Doxazosin Mesylate

HRID 389922

反応式

HRID 389922 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:14]([NH2:15])=[N:13][C:12]([N:16]3[CH2:21][CH2:20][N:19]([C:22]([CH:24]4[O:33][C:32]5[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=5[O:26][CH2:25]4)=[O:23])[CH2:18][CH2:17]3)=[N:11][C:6]2=[CH:7][C:8]=1[O:9][CH3:10].[CH3:34][S:35]([OH:38])(=[O:37])=[O:36]>CC(C)=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:14]([NH2:15])=[N:13][C:12]([N:16]3[CH2:17][CH2:18][N:19]([C:22]([CH:24]4[O:33][C:32]5[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=5[O:26][CH2:25]4)=[O:23])[CH2:20][CH2:21]3)=[N:11][C:6]2=[CH:7][C:8]=1[O:9][CH3:10].[CH3:34][S:35]([OH:38])(=[O:37])=[O:36]

参加物

4

反応物 2

HCID 3157DoxazosinHCID 6395Methanesulfonic Acid

生成物 1

HCID 62978Doxazosin Mesylate

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
27.5 °C

実験手順

Doxazosin (100 gms) was charged in acetone (0.8 lit) at room temperature. The contents were stirred for 10 mins at 25-30° C. Methane sulfonic acid (23.2 ml) was charged slowly at 25-30° C. The reaction mass was heated at 35-38° C. and the temperature maintained for 2 hours. The reaction mass was cooled to 25-30° C. and stirred for 1 hour. The solid obtained was filtered and washed with acetone (100 ml). The product was dried at 55-60° C. under vacuum to obtain pure Form IV doxazosin mesylate (115-120 gms) which was characterized by XRD, IR and DSC. Purity according to HPLC: −99.89%.

後処理

  1. temperatureThe reaction mass was heated at 35-38° C.
  2. temperaturethe temperature maintained for 2 hours
  3. temperatureThe reaction mass was cooled to 25-30° C.
  4. stirringstirred for 1 hour
  5. customThe solid obtained
  6. filtrationwas filtered
  7. washwashed with acetone (100 ml)
  8. customThe product was dried at 55-60° C. under vacuum

出典と根拠

ORDレコード
ord-1a6ba6391c4d48a987c1572417db0707
出典データセット
uspto-grants-2013_02
特許番号
US08383627B2

関連ノート

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