N,N,N-trimethyl-1,1-bis(1-methylethoxy)amine → [2-(4-Bromo-5-fluoro-2-nitro-phenyl)-vinyl]-dimethyl-amine

HRID 489717노트

반응식

HRID 489717 반응식
C(O[CH:5](OC(C)C)[N:6]([CH3:8])[CH3:7])(C)C.[Br:13][C:14]1[CH:19]=[C:18]([N+:20]([O-:22])=[O:21])[C:17]([CH3:23])=[CH:16][C:15]=1[F:24]>CN(C)C=O>[Br:13][C:14]1[C:15]([F:24])=[CH:16][C:17]([CH:23]=[CH:5][N:6]([CH3:7])[CH3:8])=[C:18]([N+:20]([O-:22])=[O:21])[CH:19]=1

참가 물질

4

반응물 2

HCID 87682N,N,N-trimethyl-1,1-bis(1-methylethoxy)amineHCID 27793654-Bromo-5-fluoro-2-nitrotoluene

생성물 1

HCID 73878710[2-(4-Bromo-5-fluoro-2-nitro-phenyl)-vinyl]-dimethyl-amine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
122.5 °C

실험 절차

A mixture of N,N-dimethyl formamide diisopropyl acetal (1.7 ml, 8.13 mmol) and 1-Bromo-2-fluoro-4-methyl-5-nitro-benzene (1.538 g, 6.57 mmoles) in dry dimethylformamide (10 ml) was heated at 120-125° C. for 1.5 hours. The resulting dark red solution was concentrated under reduced pressure and partitioned between ethyl acetate and water. The organic extract was washed with brine, dried (anhydrous sodium sulfate), and concentrated under reduced pressure to give [2-(4-Bromo-5-fluoro-2-nitro-phenyl)-vinyl]-dimethyl-amine as a dark red solid.

후처리

  1. concentrationThe resulting dark red solution was concentrated under reduced pressure
  2. custompartitioned between ethyl acetate and water
  3. extractionThe organic extract
  4. washwas washed with brine
  5. dry with materialdried (anhydrous sodium sulfate)
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-f0aa0231728c40fcbf827b2f84b2a979
출처 데이터셋
uspto-grants-2005_12
특허 번호
US06979696B2

반응 노트

불러오는 중…