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Thionyl Chloride → HCID 22030137, 화합물

HRID 968620
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HRID 968620 반응식
[N+:1]([C:4]1[C:9](=O)[NH:8][CH:7]=[C:6]([C:11]2[C:16]([C:17]([F:20])([F:19])[F:18])=[CH:15][CH:14]=[CH:13][N:12]=2)[CH:5]=1)([O-:3])=[O:2].S(Cl)([Cl:23])=O>CN(C=O)C>[Cl:23][C:9]1[N:8]=[CH:7][C:6]([C:11]2[C:16]([C:17]([F:20])([F:19])[F:18])=[CH:15][CH:14]=[CH:13][N:12]=2)=[CH:5][C:4]=1[N+:1]([O-:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 22030083HCID 22030083, 화합물

생성물 1

HCID 22030137HCID 22030137, 화합물수율 93%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Heat a solution of 5′-nitro-3-trifluoromethyl-1′H-[2,3′]bipyridinyl-6′-one (25 g, 0.088 mol), thionyl chloride (300 mL) and DMF (3 mL) to reflux for 4 hours. Remove the volatiles by rotary evaporation and partition the residue between ethyl acetate (350 mL) and saturated sodium bicarbonate solution (250 mL). Extract the aqueous layer with further ethyl acetate (250 mL) and wash the combined organics with brine (250 mL). Dry (MgSO4) and concentrate under reduced pressure to give the title compound (25 g, 93%) as a yellow oil.

후처리

  1. temperatureto reflux for 4 hours
  2. customRemove the volatiles
  3. customby rotary evaporation
  4. custompartition the residue between ethyl acetate (350 mL) and saturated sodium bicarbonate solution (250 mL)
  5. extractionExtract the aqueous layer with further ethyl acetate (250 mL)
  6. washwash the combined organics with brine (250 mL)
  7. dry with materialDry (MgSO4)
  8. concentrationconcentrate under reduced pressure

출처 및 근거

ORD 기록
ord-1e92cbde95014a5b9c0a1bea95a649da
출처 데이터셋
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07304059B2

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