Batefenterol → Batefenterol edisylate

HRID 407127노트

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HRID 407127 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([CH2:8][NH:9][CH2:10][C@H:11]([OH:24])[C:12]2[CH:21]=[CH:20][C:19]([OH:22])=[C:18]3[C:13]=2[CH:14]=[CH:15][C:16](=[O:23])[NH:17]3)[C:5]([O:25][CH3:26])=[CH:4][C:3]=1[NH:27][C:28]([CH2:30][CH2:31][N:32]1[CH2:37][CH2:36][CH:35]([O:38][C:39](=[O:53])[NH:40][C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][C:42]=2[C:47]2[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=2)[CH2:34][CH2:33]1)=[O:29].O.O.[CH2:56]([S:62]([OH:65])(=[O:64])=[O:63])[CH2:57][S:58]([OH:61])(=[O:60])=[O:59]>C(O)(C)C.O>[CH2:56]([S:62]([OH:65])(=[O:64])=[O:63])[CH2:57][S:58]([OH:61])(=[O:60])=[O:59].[Cl:1][C:2]1[CH:7]=[C:6]([CH2:8][NH:9][CH2:10][C@H:11]([OH:24])[C:12]2[CH:21]=[CH:20][C:19]([OH:22])=[C:18]3[C:13]=2[CH:14]=[CH:15][C:16](=[O:23])[NH:17]3)[C:5]([O:25][CH3:26])=[CH:4][C:3]=1[NH:27][C:28]([CH2:30][CH2:31][N:32]1[CH2:37][CH2:36][CH:35]([O:38][C:39](=[O:53])[NH:40][C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][C:42]=2[C:47]2[CH:48]=[CH:49][CH:50]=[CH:51][CH:52]=2)[CH2:34][CH2:33]1)=[O:29]

참가 물질

5

반응물 2

HCID 10372836BatefenterolHCID 57346009Ethane-1,2-disulfonic acid--water (1/2)

생성물 1

HCID 11629376Batefenterol edisylate수율 95.5%

시약·촉매·용매 2

HCID 962Water용매HCID 3776Isopropanol용매

실험 절차

Biphenyl-2-ylcarbamic acid 1-[2-(2-chloro-4-{[(r)-2-hydroxy-2-(8-hydroxy-2-oxo-1,2-dihydroquinolin-5-yl)ethylamino]methyl}-5-methoxyphenylcarbamoyl)-ethyl]piperidin-4-yl ester (5 g, 6.75 mmol, >99% pure) was dissolved in isopropanol (100 mL), followed by addition of ethane disulfonic acid dihydrate (1.525 mg, 6.75 mmol) dissolved in water (20 mL). The resulting slurry was stirred at room temperature for 1 hour, and then at ˜30° C. overnight. The title compound (6.0 g) was isolated as a white powder. The product was heated in 20% water in isopropanol (100 mL) at 30° C. for 48 hours. After cooling to room temperature, the resulting precipitate was isolated by filtration and dried in air for 2 hours to yield the title compound (5.4 g).

후처리

  1. customat ˜30° C.
  2. customovernight

출처 및 근거

ORD 기록
ord-1c27780120a3466b96db4c0a63028356
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08754223B2

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