Terazosin Hydrochloride → Terazosin

HRID 2379399

반응식

HRID 2379399 반응식
[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]

참가 물질

3

반응물 1

HCID 63016Terazosin Hydrochloride

생성물 1

HCID 5401Terazosin

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c6467a64a2334146a6dbff801f20d4a7
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05362730

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