Terazosin Hydrochloride → Terazosin

HRID 2379400ノート

反応式

HRID 2379400 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]2[C:9]([NH2:26])=[N:10][C:11]([N:13]3[CH2:18][CH2:17][N:16]([C:19]([CH:21]4[O:25][CH2:24][CH2:23][CH2:22]4)=[O:20])[CH2:15][CH2:14]3)=[N:12][C:6]2=[CH:5][C:4]=1[O:27][CH3:28].O.O.Cl>CC(C)=O>[CH3:1][O:2][C:3]1[CH:8]=[C:7]2[C:9]([NH2:26])=[N:10][C:11]([N:13]3[CH2:18][CH2:17][N:16]([C:19]([CH:21]4[O:25][CH2:24][CH2:23][CH2:22]4)=[O:20])[CH2:15][CH2:14]3)=[N:12][C:6]2=[CH:5][C:4]=1[O:27][CH3:28]

参加物

3

反応物 1

HCID 63016Terazosin Hydrochloride

生成物 1

HCID 5401Terazosin収率 90.9%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a 500-mL round-bottom flask containing 5.19 g (0.011 mol) of terazosin monohydrochloride dihydrate was added 250 mL of dry acetone and several glass boiling beads. The flask was fitted with a Dean-Stark trap and reflux condensor. The heterogenous mixture was heated under reflux for five days. After cooling, the undissolved white solid remaining in the flask was collected by vacuum filtration to yield 4.3 g (0.010 mol, 90.9% yield) of the anhydrous crystalline polymorph of terazosin of this invention. The material was found by its powder x-ray diffraction pattern to be free of both the prior art anhydrous crystalline modification and the dihydrate form.

後処理

  1. customThe flask was fitted with a Dean-Stark trap
  2. temperaturereflux condensor
  3. temperatureThe heterogenous mixture was heated
  4. temperatureunder reflux for five days
  5. temperatureAfter cooling
  6. filtrationwas collected by vacuum filtration

出典と根拠

ORDレコード
ord-c7aa683dcf7d443886995c02b7c0e72e
出典データセット
uspto-grants-1994_11
特許番号
US05362730

反応ノート

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