Tert-Butylamine → Perindopril Erbumine

HRID 273475

반응식

HRID 273475 반응식
[CH3:1][CH2:2][CH2:3][C@H:4]([NH:10][C@H:11]([C:13]([N:15]1[C@H:23]([C:24]([OH:26])=[O:25])[CH2:22][C@H:21]2[C@@H:16]1[CH2:17][CH2:18][CH2:19][CH2:20]2)=[O:14])[CH3:12])[C:5]([O:7][CH2:8][CH3:9])=[O:6].C(OCC)(=O)C.[C:33]([NH2:37])([CH3:36])([CH3:35])[CH3:34]>COC(OC)(C)C>[CH3:1][CH2:2][CH2:3][C@H:4]([NH:10][C@H:11]([C:13]([N:15]1[C@H:23]([C:24]([OH:26])=[O:25])[CH2:22][C@H:21]2[C@@H:16]1[CH2:17][CH2:18][CH2:19][CH2:20]2)=[O:14])[CH3:12])[C:5]([O:7][CH2:8][CH3:9])=[O:6].[CH3:34][C:33]([NH2:37])([CH3:36])[CH3:35]

참가 물질

5

반응물 3

HCID 6385Tert-ButylamineHCID 8857Ethyl AcetateHCID 107807Perindopril

생성물 1

HCID 441313Perindopril Erbumine

시약·촉매·용매 1

HCID 64952,2-Dimethoxypropane용매

실험 절차

Perindopril (I) prepared exactly as per the method described in our pending PCT Application No. PCT/IN03/00042, dated Feb. 28, 2003 and as per the chemistry summarized in Scheme-II and as mentioned hereinbefore in Section 1 (b) was suspended in 2,2-dimethoxypropane (instead of ethyl acetate) to which was gradually tertiary-butylamine. The mixture was heated to reflux till a clear solution was obtained and filtered hot to remove any suspended particles. Thereafter, the solution was cooled to 20° C. to 30° C., and then further cooled to 0° C. to 15° C., maintained at the same temperature for 30 minutes to 1 hour and finally the crystallized solid was filtered and dried at 40-45° C. under vacuum for 5-6 hours to give crystalline perindopril erbumine (IU), exhibiting IR spectra values and, DSC thermogram summarized hereinbelow

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux till a clear solution
  3. customwas obtained
  4. filtrationfiltered hot
  5. customto remove any suspended particles
  6. temperatureThereafter, the solution was cooled to 20° C. to 30° C.
  7. temperaturefurther cooled to 0° C. to 15° C.
  8. temperaturemaintained at the same temperature for 30 minutes to 1 hour
  9. filtrationfinally the crystallized solid was filtered
  10. customdried at 40-45° C. under vacuum for 5-6 hours

출처 및 근거

ORD 기록
ord-45c68e6b42f54ec8bec624d6832c614b
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07456296B2

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