Water → Benzenamine, 5-methoxy-N-methyl-2-nitro-

HRID 33391

반응식

HRID 33391 반응식
[CH3:1][NH2:2].F[C:4]1[CH:5]=[C:6]([O:13][CH3:14])[CH:7]=[CH:8][C:9]=1[N+:10]([O-:12])=[O:11].C(=O)([O-])[O-].[K+].[K+].O>C1COCC1.ClCCl>[CH3:14][O:13][C:6]1[CH:7]=[CH:8][C:9]([N+:10]([O-:12])=[O:11])=[C:4]([NH:2][CH3:1])[CH:5]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 6329MethylamineHCID 11430Potassium CarbonateHCID 5656543-Fluoro-4-nitroanisole

생성물 1

HCID 153056Benzenamine, 5-methoxy-N-methyl-2-nitro-

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

83.5 mL (167.0 mmol) of a 2 molar solution of methylamine in THF are added dropwise to 14.3 g (83.56 mmol) 3-fluoro-4-nitro-anisol and 12.71 g (92.02 mmol) potassium carbonate in 200 mL dichloromethane. The mixture is stirred overnight and then combined with water. The organic phase is washed successively with water and ammonium chloride solution, dried and evaporated down. The yellow solid remaining is stirred with hexane. Yield: 12.7 g (84%); mass spectroscopy: [M+H]+=183.

후처리

  1. washThe organic phase is washed successively with water and ammonium chloride solution
  2. customdried
  3. customevaporated down
  4. stirringThe yellow solid remaining is stirred with hexane

출처 및 근거

ORD 기록
ord-bc918e6a5f98444a864a487a48b4fb21
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429583B2

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