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Hydrochloric Acid → HCID 71735460, 화합물

HRID 1481234
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인쇄 미리보기

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HRID 1481234 반응식
Cl.[NH2:2][CH2:3][CH:4]([C:8]1[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=1)[C:5]([OH:7])=[O:6].C[O:16][C:17]([C:19]1[N:20]=[CH:21][C:22]2[C:27]([C:28]=1[OH:29])=[CH:26][CH:25]=[C:24]([O:30][C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)[CH:23]=2)=O.C[O-].[Na+].C[C:41]([N:43](C)C)=O>>[C:41]([C:21]1[C:22]2[C:27](=[CH:26][CH:25]=[C:24]([O:30][C:31]3[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=3)[CH:23]=2)[C:28]([OH:29])=[C:19]([C:17]([NH:2][CH2:3][CH:4]([C:8]2[CH:9]=[CH:10][C:11]([F:14])=[CH:12][CH:13]=2)[C:5]([OH:7])=[O:6])=[O:16])[N:20]=1)#[N:43]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 5

HCID 313Hydrochloric AcidHCID 31374DimethylacetamideHCID 10942334Sodium MethoxideHCID 22339844α-(Aminomethyl)-4-fluorobenzeneacetic acidHCID 86709142Methyl 4-hydroxy-7-phenoxyisoquinoline-3-carboxylate

생성물 1

HCID 71735460HCID 71735460, 화합물

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온도
150 °C

실험 절차

A mixture of HCl salt of 3-amino-2-(4-fluoro-phenyl)-propionic acid (82 mg), 4-hydroxy-7-phenoxy-isoquinoline-3-carboxylic acid methyl ester (40 mg) and NaOMe (41 mg) in DMA (1 mL) was heated in an oil bath (150° C.) for 1 h. The reaction mixture was then partitioned between EtOAc and diluted HCl solution, EtOAc phase was separated and washed with water, diluted NaCl solution and dried over anhydrous sodium sulfate solution, filtered, concentrated and silica gel column column-purified to give desired product (19 mg). LC-MS ESI+: 472 (M+1)+.

후처리

  1. customThe reaction mixture was then partitioned between EtOAc and diluted HCl solution, EtOAc phase
  2. customwas separated
  3. washwashed with water, diluted NaCl solution
  4. dry with materialdried over anhydrous sodium sulfate solution
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customsilica gel column column-purified

출처 및 근거

ORD 기록
ord-c679699359c54561a966d086d75d9e31
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09409892B2

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