Water → 3-Methoxy-4-nitrobenzonitrile

HRID 1511837노트

반응식

HRID 1511837 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][C:11]=1[N+:12]([O-:14])=[O:13])[C:6]([NH2:8])=O.N1C=CC=CC=1.FC(F)(F)C(OC(=O)C(F)(F)F)=O.O>O1CCOCC1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][C:11]=1[N+:12]([O-:14])=[O:13])[C:6]#[N:8]

참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 9845Trifluoroacetic anhydrideHCID 110633383-Methoxy-4-nitrobenzamide

생성물 1

HCID 108992273-Methoxy-4-nitrobenzonitrile

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a solution of 3-methoxy-4-nitrobenzamide (8 g, 41 mmol) in dioxane (300 mL) was added pyridine (32 g, 408 mmol), followed by dropwise addition of trifluoroacetic anhydride (43 g, 204 mmol). The reaction mixture was stirred at room temperature for 5 h. Water was added to quench the reaction. The mixture was concentrated, then the residue was partitioned between ethyl acetate and water. The organic layer was separated, the aqueous layer was extracted with ethyl acetate. The organic layers were combined, washed with water, aqueous saturated CuSO4 solution, brine, dried over MgSO4, and concentrated to give 3-methoxy-4-nitrobenzonitrile as a off white solid (6.5 g, 90%)

후처리

  1. customto quench
  2. customthe reaction
  3. concentrationThe mixture was concentrated
  4. customthe residue was partitioned between ethyl acetate and water
  5. customThe organic layer was separated
  6. extractionthe aqueous layer was extracted with ethyl acetate
  7. washwashed with water, aqueous saturated CuSO4 solution, brine
  8. dry with materialdried over MgSO4
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1ce235f726f643b6840bf88b14ef2b93
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217044B2

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