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Lithium Hydroxide → HCID 56589687, 화합물

HRID 1889202
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HRID 1889202 반응식
C[O:2][C:3](=[O:41])[C:4]1[CH:9]=[CH:8][C:7]([O:10][C:11]2[S:15][C:14]([NH:16][C:17](=[O:40])[CH:18]([C:28]3[CH:33]=[CH:32][C:31]([S:34]([CH:37]4[CH2:39][CH2:38]4)(=[O:36])=[O:35])=[CH:30][CH:29]=3)[O:19][C:20]3[CH:25]=[CH:24][C:23]([F:26])=[CH:22][C:21]=3[F:27])=[N:13][CH:12]=2)=[CH:6][CH:5]=1.[Li+].[OH-]>C1COCC1.CO>[CH:37]1([S:34]([C:31]2[CH:30]=[CH:29][C:28]([CH:18]([O:19][C:20]3[CH:25]=[CH:24][C:23]([F:26])=[CH:22][C:21]=3[F:27])[C:17]([NH:16][C:14]3[S:15][C:11]([O:10][C:7]4[CH:6]=[CH:5][C:4]([C:3]([OH:41])=[O:2])=[CH:9][CH:8]=4)=[CH:12][N:13]=3)=[O:40])=[CH:33][CH:32]=2)(=[O:35])=[O:36])[CH2:38][CH2:39]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 56592434HCID 56592434, 화합물

생성물 1

HCID 56589687HCID 56589687, 화합물수율 86%

시약·촉매·용매 1

HCID 21899815MeOH tetrahydrofuran용매

실험 절차

4-{2-[2-(4-Cyclopropanesulfonyl-phenyl)-2-(2,4-difluoro-phenoxy)-acetylamino]thiazol-5-yloxy}-benzoic acid methyl ester (1.4 g, 2.33 mmol, obtained in example A74) was taken in THF: MeOH (1:1, 20 mL), to it was added aqueous solution of LiOH (0.34 g, 7.94 mmol in 10 mL water) and stirred for 1-4 h. After completion of the reaction, organic solvent was removed under reduced pressure. The aqueous layer was washed with diisopropyl ether then acidified with 1 N HCl to pH 2. The solid formed was filtered, washed with water, followed by washing with diisopropyl ether & dried under vacuum to get the title compound (1.17 g, 86%).

후처리

  1. customAfter completion of the reaction, organic solvent
  2. customwas removed under reduced pressure
  3. washThe aqueous layer was washed with diisopropyl ether
  4. customThe solid formed
  5. filtrationwas filtered
  6. washwashed with water
  7. washby washing with diisopropyl ether
  8. customdried under vacuum

출처 및 근거

ORD 기록
ord-3285287352e1424f89cd6af69ac263bf
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08501955B2

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