Methanol → Octreotide

HRID 1797776노트

반응식

HRID 1797776 반응식
[CH3:1][C@@H:2]([OH:71])[C@@H:3]1[NH:27][C:25](=[O:26])[C@H:24]([CH2:28][CH2:29][CH2:30][CH2:31][NH2:32])[NH:23][C:21](=[O:22])[C@@H:20]([CH2:33][C:34]2[C:38]3[CH:39]=[CH:40][CH:41]=[CH:42][C:37]=3[NH:36][CH:35]=2)[NH:19][C:17](=[O:18])[C@H:16]([CH2:43][C:44]2[CH:45]=[CH:46][CH:47]=[CH:48][CH:49]=2)[NH:15][C:13](=[O:14])[C@@H:12]([NH:50][C:51]([C@H:53]([NH2:61])[CH2:54][C:55]2[CH:56]=[CH:57][CH:58]=[CH:59][CH:60]=2)=[O:52])[CH2:11][S:10][S:9][CH2:8][C@@H:7]([C:62]([NH:64][C@@H:65]([C@H:68]([OH:70])[CH3:69])[CH2:66][OH:67])=[O:63])[NH:6][C:4]1=[O:5].C(Cl)Cl.C[OH:76]>>[CH3:1][C@@H:2]([OH:71])[C@@H:3]1[NH:27][C:25](=[O:26])[C@H:24]([CH2:28][CH2:29][CH2:30][CH2:31][NH2:32])[NH:23][C:21](=[O:22])[C@@H:20]([CH2:33][C:34]2[C:38]3[CH:39]=[CH:40][CH:41]=[CH:42][C:37]=3[NH:36][CH:35]=2)[NH:19][C:17](=[O:18])[C@H:16]([CH2:43][C:44]2[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=2)[NH:15][C:13](=[O:14])[C@@H:12]([NH:50][C:51]([C@H:53]([NH2:61])[CH2:54][C:55]2[CH:60]=[CH:59][CH:58]=[CH:57][CH:56]=2)=[O:52])[CH2:11][S:10][S:9][CH2:8][C@@H:7]([C:62]([NH:64][C@@H:65]([C@H:68]([OH:70])[CH3:69])[CH2:66][OH:67])=[O:63])[NH:6][C:4]1=[O:5].[CH3:1][C@@H:2]([OH:71])[C@@H:3]1[NH:27][C:25](=[O:26])[C@H:24]([CH2:28][CH2:29][CH2:30][CH2:31][NH2:32])[NH:23][C:21](=[O:22])[C@@H:20]([CH2:33][C:34]2[C:38]3[CH:39]=[CH:40][CH:41]=[CH:42][C:37]=3[NH:36][CH:35]=2)[NH:19][C:17](=[O:18])[C@H:16]([CH2:43][C:44]2[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=2)[NH:15][C:13](=[O:14])[C@@H:12]([NH:50][C:51]([C@H:53]([NH2:61])[CH2:54][C:55]2[CH:60]=[CH:59][CH:58]=[CH:57][CH:56]=2)=[O:52])[CH2:11][S:10][S:9][CH2:8][C@@H:7]([C:62]([NH:64][C@@H:65]([C@H:68]([OH:70])[CH3:69])[CH2:66][OH:67])=[O:63])[NH:6][C:4]1=[O:5].[CH3:69][C:68]([OH:70])=[O:76]

참가 물질

5

반응물 3

HCID 887MethanolHCID 6344DichloromethaneHCID 448601Octreotide

생성물 2

HCID 448601OctreotideHCID 6917964Octreotide xAcetate

실험 절차

Various Octreotide microspheres were prepared from a clear dispersed phase containing the polymer, octreotide, methylene chloride (DCM) and methanol. Octreotide acetate was obtained from Polypeptide Laboratories or Peninsula Lab. Polymer concentration was varied for the batches to obtain appropriate particle size and also to obtain efficient drug load. Methanol (MeOH) to DCM ratio was increased while making higher drug load batches to get a clear dispersed phase. The continuous phase was a 0.35% PVA solution in all preparations. In a typical preparation, CP was taken in a beaker and stirred using a Silverson homogenizer (standard emulsor screen). To the stirring CP, the dispersed phase was added just below the Silverson head using a laboratory syringe with a bent needle. After 30 sec to 1 minute homogenization, the entire suspension was transferred into a 3 liter Applikon bioreactor for solvent removal. The solvent removal from the microsphere was achieved by initial CP replacement with water followed by heating the suspension at 40° C. along with air sweep. After the solvent removal the microspheres were collected on a filter membrane, washed and dried under vacuum.

출처 및 근거

ORD 기록
ord-21e9a5da84824cadaf1504fcdf95c23a
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08343513B2

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