Nitronium tetrafluoroborate → HCID 19895665, 화합물

HRID 1073878노트

반응식

HRID 1073878 반응식
[CH3:1][C:2]1([CH3:19])[CH2:7][CH:6]([C:8]2[C:13]([CH3:14])=[CH:12][CH:11]=[CH:10][N:9]=2)[C:5]2[CH:15]=[CH:16][CH:17]=[CH:18][C:4]=2[O:3]1.F[B-](F)(F)F.[O:25]=[N+:26]=[O:27]>C(#N)C>[CH3:1][C:2]1([CH3:19])[CH2:7][CH:6]([C:8]2[C:13]([CH3:14])=[CH:12][CH:11]=[CH:10][N:9]=2)[C:5]2[CH:15]=[C:16]([N+:26]([O-:27])=[O:25])[CH:17]=[CH:18][C:4]=2[O:3]1

참가 물질

4

반응물 2

HCID 11073463Nitronium tetrafluoroborateHCID 19895670HCID 19895670, 화합물

생성물 1

HCID 19895665HCID 19895665, 화합물수율 46.4%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

685 mg of 3,4-dihydro-2,2-dimethyl-4-(3-methyl-2-pyridyl)-2H-1-benzopyran were dissolved in 20 ml of acetonitrile at room temperature and 360 mg of nitronium tetrafluoroborate were added. After 30 minutes the solvent was removed by evaporation and ethyl acetate and water were added. The organic phase was dried over sodium sulphate and evaporated. The residue was chromatographed on silica gel using ethyl acetate/petroleum ether (1:4) for the elution. There were obtained 374 mg of 3,4-dihydro-2,2-dimethyl-4-(3-methyl-2-pyridyl) -6-nitro-2H-1-benzopyran in the form of a solid of melting pOint 164-165° C. after recrystallization from t-butyl methyl ether.

후처리

  1. customAfter 30 minutes the solvent was removed by evaporation and ethyl acetate and water
  2. additionwere added
  3. dry with materialThe organic phase was dried over sodium sulphate
  4. customevaporated
  5. customThe residue was chromatographed on silica gel
  6. washfor the elution

출처 및 근거

ORD 기록
ord-edd95b701db0438ba99668e1e19dcf25
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04971982

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