Potassium Nitrate → 5,5-dimethyl-8-nitro-2,3,4,5-tetrahydro-1H-benzo[b]azepine

HRID 401380노트

반응식

HRID 401380 반응식
[N+:1]([O-:4])([O-])=[O:2].[K+].[CH3:6][C:7]1([CH3:18])[CH2:13][CH2:12][CH2:11][NH:10][C:9]2[CH:14]=[CH:15][CH:16]=[CH:17][C:8]1=2.C([O-])(O)=O.[Na+]>OS(O)(=O)=O>[CH3:6][C:7]1([CH3:18])[CH2:13][CH2:12][CH2:11][NH:10][C:9]2[CH:14]=[C:15]([N+:1]([O-:4])=[O:2])[CH:16]=[CH:17][C:8]1=2

참가 물질

5

반응물 3

HCID 24434Potassium NitrateHCID 516892Sodium BicarbonateHCID 574702555,5-dimethyl-2,3,4,5-tetrahydro-1H-1-benzazepine

생성물 1

HCID 574702565,5-dimethyl-8-nitro-2,3,4,5-tetrahydro-1H-benzo[b]azepine수율 86.8%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

At 0° C., KNO3 (0.76 g, 7.54 mmol) was added portionwise to a solution of 5,5-dimethyl-2,3,4,5-tetrahydro-1H-benzo[b]azepine (1.1 g, 6.28 mmol) in H2SO4 (15 mL). After stifling 15 min at this temperature, the mixture was poured into ice water, basified with sat. NaHCO3 to pH 8 and extracted with EtOAc. The organic layer was washed with brine, dried over Na2SO4 and concentrated to give crude 5,5-dimethyl-8-nitro-2,3,4,5-tetrahydro-1H-benzo[b]azepine (1.2 g), which was used directly in the next step without further purification.

후처리

  1. extractionextracted with EtOAc
  2. washThe organic layer was washed with brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3032f45f7d6949cc91f4fff22ba8e27f
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08741925B2

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