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Sodium Hydroxide → HCID 178525891, 화합물

HRID 1746226
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HRID 1746226 반응식
C([O:3][C:4](=[O:28])[CH2:5][NH:6][C:7]([C:9]1[C:10](=[O:27])[S:11][C:12]2[C:17]([C:18]=1[OH:19])=[CH:16][C:15]([Cl:20])=[CH:14][C:13]=2[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)=[O:8])C.[OH-].[Na+]>C1COCC1.CO>[Cl:20][C:15]1[CH:16]=[C:17]2[C:12](=[C:13]([C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)[CH:14]=1)[S:11][C:10](=[O:27])[C:9]([C:7]([NH:6][CH2:5][C:4]([OH:28])=[O:3])=[O:8])=[C:18]2[OH:19]
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 178472765HCID 178472765, 화합물

생성물 1

HCID 178525891HCID 178525891, 화합물수율 94.8%

시약·촉매·용매 1

HCID 21899815MeOH tetrahydrofuran용매

실험 절차

[(6-Chloro-4-hydroxy-2-oxo-8-phenyl-2H-thiochromene-3-carbonyl)-amino]-acetic acid ethyl ester (200 mg, 0.479 mmol) was dissolved in THF-Methanol (1:1; 13 mL total volume.) Sodium hydroxide (1.5 mmol, 1.5 mL; 1M) was added and the solution stirred overnight at ambient temperature. The reaction mixture was concentrated in vacuo and the residue was dissolved in water (10 mL.) The crude product was precipitated with 1N HCl (3 mL) and isolated via filtration and triturated with hexanes to provide the title compound (177 mg.) MS ESI(+) m/e: 390.118, 392.226 (M+1).

후처리

  1. additionwas added
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. dissolutionthe residue was dissolved in water (10 mL.) The crude product
  4. customwas precipitated with 1N HCl (3 mL)
  5. customisolated via filtration
  6. customtriturated with hexanes

출처 및 근거

ORD 기록
ord-d1ba6dc41e724cff89b2202c46880cbb
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09149476B2

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