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

HRID 489717ノート

反応式

HRID 489717 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
122.5 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f0aa0231728c40fcbf827b2f84b2a979
出典データセット
uspto-grants-2005_12
特許番号
US06979696B2

反応ノート

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