Ethyl Acetate → HCID 7172095, 화합물

HRID 1844606노트

반응식

HRID 1844606 반응식
F[B-](F)(F)F.[O:6]=[N+:7]=[O:8].[C:9]([C:13]1[CH:14]=[CH:15][C:16]([OH:21])=[C:17]([CH:20]=1)[CH:18]=[O:19])([CH3:12])([CH3:11])[CH3:10].C(OCC)(=O)C.C([O-])(O)=O.[Na+]>C(#N)C>[C:9]([C:13]1[CH:14]=[C:15]([N+:7]([O-:8])=[O:6])[C:16]([OH:21])=[C:17]([CH:20]=1)[CH:18]=[O:19])([CH3:12])([CH3:10])[CH3:11]

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 516892Sodium BicarbonateHCID 14750905-tert-ButylsalicylaldehydeHCID 11073463Nitronium tetrafluoroborate

생성물 1

HCID 7172095HCID 7172095, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
-15 °C

실험 절차

At −30° C. 4.84 g nitroniumtetrafluoroborate are added to a solution of 5.00 g 5-tert-butyl-2-hydroxy-benzaldehyde in 200 ml acetonitrile. The solution is heated to −15° C. within 1 h and then combined with ethyl acetate and saturated aqueous NaHCO3 solution. The resulting mixture is extracted with ethyl acetate, and the combined extracts are washed with saturated aqueous saline solution, dried (MgSO4) and evaporated down. The residue is taken up in 2 ml of water and 40 ml concentrated acetic acid, and the resulting mixture is refluxed for 2 h. The cooled solution is poured into ice-cold water, and the precipitate formed is filtered off and dissolved in ethyl acetate. The organic solution is dried (MgSO4) and evaporated down. The oil remaining rapidly solidifies.

후처리

  1. customAt −30° C
  2. extractionThe resulting mixture is extracted with ethyl acetate
  3. washthe combined extracts are washed with saturated aqueous saline solution
  4. dry with materialdried (MgSO4)
  5. customevaporated down
  6. temperature40 ml concentrated acetic acid, and the resulting mixture is refluxed for 2 h
  7. additionThe cooled solution is poured into ice-cold water
  8. customthe precipitate formed
  9. filtrationis filtered off
  10. dissolutiondissolved in ethyl acetate
  11. dry with materialThe organic solution is dried (MgSO4)
  12. customevaporated down

출처 및 근거

ORD 기록
ord-7fad12f122484f8f96a1237ed039aa89
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946438B2

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