Terazosin Hydrochloride → Terazosin

HRID 2379399

反応式

HRID 2379399 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>C(O)C>[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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a 2-liter round-bottom flask containing 71.0 g (0.15 mol) of terazosin monohydrochloride dihydrate was added 1300 mL of absolute ethanol, a stirring bar 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 two days. After cooling, the undissolved white solid remaining in the flask was collected by vacuum filtration and washed with dry acetone to yield 60.9 g (0.143 mol, 93.5%) 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 two days
  5. temperatureAfter cooling
  6. filtrationwas collected by vacuum filtration
  7. washwashed with dry acetone

出典と根拠

ORDレコード
ord-c6467a64a2334146a6dbff801f20d4a7
出典データセット
uspto-grants-1994_11
特許番号
US05362730

関連ノート

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