Ethanol → 5-Bromo-2-(tetrahydropyran-4-yl)nitrobenzene

HRID 74182

반응식

HRID 74182 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5](F)=[C:6]([N+:8]([O-:10])=[O:9])[CH:7]=1.C(N(CC)CC)C.N[CH:20]1[CH2:25][CH2:24][O:23][CH2:22][CH2:21]1.C(O)C>O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH:20]2[CH2:25][CH2:24][O:23][CH2:22][CH2:21]2)=[C:6]([N+:8]([O-:10])=[O:9])[CH:7]=1

참가 물질

6

반응물 4

HCID 702EthanolHCID 8471TriethylamineHCID 4192234-AminotetrahydropyranHCID 27363284-Bromo-1-fluoro-2-nitrobenzene

생성물 1

HCID 674988265-Bromo-2-(tetrahydropyran-4-yl)nitrobenzene수율 91.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

An eggplant flask was charged with 5-bromo-2-fluoronitrobenzene (3.0 g, 13.6 mmol), triethylamine (1.66 g, 16.3 mmol), 4-aminotetrahydropyran (1.52 g, 15.0 mmol), and ethanol (60 mL), and this was heated to reflux with stirring for 2 hours. After concentration of the reaction mixture under reduced pressure, water (60 mL) was added and this was stirred as is at room temperature for 30 minutes. The precipitated crystals were filtered off and washed with water. The crystals obtained were dried at reduced pressure with heating to yield the title compound (3.55 g, 86% yield) as a reddish-orange solid.

후처리

  1. temperaturethis was heated
  2. temperatureto reflux
  3. stirringthis was stirred
  4. waitas is at room temperature for 30 minutes
  5. filtrationThe precipitated crystals were filtered off
  6. washwashed with water
  7. customThe crystals obtained
  8. customwere dried at reduced pressure
  9. temperaturewith heating

출처 및 근거

ORD 기록
ord-3a8229f9c17741f3846e907f5ce44fc5
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829035B2

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