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1,4-Dioxane hydrochloride → HCID 58160197, 화합물

HRID 1879551
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HRID 1879551 반응식
[F:1][CH2:2][CH2:3][O:4][C:5]1[C:6]([O:22]C2CCCCO2)=[CH:7][CH:8]=[C:9]2[C:14]=1[O:13][C:12](=[O:15])[CH:11]=[C:10]2[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.O1CCOCC1.Cl>>[F:1][CH2:2][CH2:3][O:4][C:5]1[C:6]([OH:22])=[CH:7][CH:8]=[C:9]2[C:14]=1[O:13][C:12](=[O:15])[CH:11]=[C:10]2[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 204431481,4-Dioxane hydrochlorideHCID 86651375HCID 86651375, 화합물

생성물 1

HCID 58160197HCID 58160197, 화합물

실험 절차

To 8-(2-fluoroethoxy)-4-phenyl-7-(tetrahydro-2H-pyran-2-yloxy)-2H-chromen-2-one was added 1.5 mL of a 4 M HCl dioxane solution. The mixture was stirred at rt for 30 min under Ar atmosphere and concentrated. The crude product was purified with chromatography (hexane/EtOAc) to afford 8-(2-fluoroethoxy)-7-hydroxy-4-phenyl-2H-chromen-2-one (AD-C-004S-WZ01055) as a white solid (24 mg, 90%). 1H NMR (400 MHz, CDCl3) δ 8.96 (s, 1H), 7.57-7.54 (m, 3H), 7.52-7.49 (m, 2H), 7.08 (dd, J=8.8, 1.2 Hz, 1H), 6.87 (dd, J=8.8, 1.2 Hz, 1 H), 6.11 (d, J=1.2 Hz, 1H), 4.86 (m, 1H), 4.74 (m, 1H), 4.50 (m, 1H), 4.43 (m, 1H); MS (ESI) m/z 301 (M+H+), 323 (M+H+).

후처리

  1. concentrationconcentrated
  2. customThe crude product was purified with chromatography (hexane/EtOAc)

출처 및 근거

ORD 기록
ord-8a3178519bb94ad0a5d19a2176b78f04
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08318132B2

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