Water → Sumatriptan Succinate

HRID 1797389

반응식

HRID 1797389 반응식
[CH3:1][NH:2][S:3]([CH2:6][C:7]1[CH:8]=[CH:9][C:10]2[NH:15][CH:14]=[C:13]([CH2:16][CH2:17][N:18]([CH3:20])[CH3:19])[C:11]=2[CH:12]=1)(=[O:5])=[O:4].O.[C:22]([OH:29])(=[O:28])[CH2:23][CH2:24][C:25]([OH:27])=[O:26]>C(#N)C>[CH3:1][NH:2][S:3]([CH2:6][C:7]1[CH:8]=[CH:9][C:10]2[NH:15][CH:14]=[C:13]([CH2:16][CH2:17][N:18]([CH3:20])[CH3:19])[C:11]=2[CH:12]=1)(=[O:5])=[O:4].[CH2:23]([C:22]([OH:29])=[O:28])[CH2:24][C:25]([OH:27])=[O:26]

참가 물질

5

반응물 3

HCID 962WaterHCID 1110Succinic AcidHCID 5358Sumatriptan

생성물 1

HCID 59772Sumatriptan Succinate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Sumatriptan (10.0 grams), water (50.0 ml), succinic acid (3.99 grams) and acetonitrile (100.0 ml) were heated to reflux temperature. The reaction mass was stirred for 15–30 minutes at reflux and filtered in hot condition. The solvent was distilled off completely from the filtrate under reduced pressure at a temperature of below 35–45° C. Cyclohexane (100 ml) was added to the resulting residual mass and stirred for 1–2 hours at a temperature of 25–35° C. to crystallize the solid. Then the solid was filtered, washed with cyclohexane (50 ml) and on subsequent drying under vacuum at a temperature of 25–35° C. there resulted the amorphous form of Sumatriptan succinate of the invention.

후처리

  1. temperatureto reflux temperature
  2. temperatureat reflux
  3. filtrationfiltered in hot condition
  4. distillationThe solvent was distilled off completely from the filtrate under reduced pressure at a temperature of below 35–45° C
  5. additionCyclohexane (100 ml) was added to the resulting residual mass
  6. stirringstirred for 1–2 hours at a temperature of 25–35° C.
  7. customto crystallize the solid
  8. filtrationThen the solid was filtered
  9. washwashed with cyclohexane (50 ml)
  10. customon subsequent drying under vacuum at a temperature of 25–35° C.

출처 및 근거

ORD 기록
ord-45b04b78ce9c47cbb51f67d772a3c1ec
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07034162B2

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