Ammonia → Sumatriptan

HRID 1625661

반응식

HRID 1625661 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].C(C(O)=O)CC(O)=O.N[C@H](C(O)=O)CC(C)C.[Na][Na].N>O>[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]

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 6106L-Leucine2회HCID 59772Sumatriptan Succinate2회HCID 141233Disodium

생성물 1

HCID 5358Sumatriptan수율 40%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Powder preparation and characterization: Sumatriptan-Na2FDKP powder was prepared as described in Example 9 above, except that the sumatriptan succinate was purchase from LGM Pharma (Boca Raton, Fla.) and L-leucine was added to study whether the aerodynamic performance of the resulting spray-dried powder formed would be improved. Three feed solutions were prepared at 4.5% total solids concentration for a 5 g scale. The feed solutions were prepared by adding FDKP disodium salt, sumatriptan succinate, and L-leucine (0-20 wt %) to de-ionized water with mixing. The solutions were titrated with dilute aqueous ammonia to pH 6.00. The resulting clear feed solutions were vacuum filtered through a 0.2 μm PES filter membrane and spray dried as described in Example 9, however, the drying gas flow was set at 25 kg/hr, the atomization flow was about 4 kg/hr and the atomization pressure was set at 4 bar. The sumatriptan succinate concentration (dry basis) in each solution was 56% to obtain a 40% sumatriptan target load. The powders were analyzed by HPLC, cascade impaction, Karl Fischer titration, scanning electron microscopy (SEM) and tap and bulk density. The results of these studies are shown in Table 9 and FIG. 22.

후처리

  1. customPowder preparation and characterization
  2. additionwas added
  3. customspray-dried powder
  4. customformed would
  5. customThe feed solutions were prepared
  6. additionwith mixing
  7. filtrationfiltered through a 0.2 μm PES
  8. filtrationfilter membrane and spray
  9. customdried
  10. concentrationThe sumatriptan succinate concentration (dry basis) in each solution

출처 및 근거

ORD 기록
ord-6eca47d641eb48239d68e7c78ae09e28
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785396B2

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