Ammonia → 4,5-Diethoxy-3-fluorophthalonitrile

HRID 1295949ノート

反応式

HRID 1295949 の反応式
Br[C:2]1[CH:7]=[C:6]([O:8][CH2:9][CH3:10])[C:5]([O:11][CH2:12][CH3:13])=[C:4]([F:14])[C:3]=1Br.[Cu](C#N)[C:17]#[N:18].N.[CH3:22][N:23](C)C=O>>[CH2:12]([O:11][C:5]1[C:4]([F:14])=[C:3]([C:22]#[N:23])[C:2](=[CH:7][C:6]=1[O:8][CH2:9][CH3:10])[C:17]#[N:18])[CH3:13]

参加物

5

反応物 4

HCID 222AmmoniaHCID 6228DimethylformamideHCID 117098891,2-Dibromo-4,5-diethoxy-3-fluorobenzeneHCID 178418260HCID 178418260、化合物

生成物 1

HCID 229298414,5-Diethoxy-3-fluorophthalonitrile

反応条件

温度
150 °C

実験手順

After dissolving the 1,2-dibromo-4,5-diethoxy-3-fluorobenzene (480 g) in dimethylformamide (1400 ml), copper cyanide (345 g) was added and the mixture was stirred at 150° C. for 3 hours. Saturated aqueous ammonia was added to the reaction mixture, and then the mixture was stirred overnight and extraction was performed with toluene. The organic layer was dried over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to yield the title compound (513 g) as white crystals.

後処理

  1. additionwas added
  2. stirringthe mixture was stirred overnight
  3. extractionextraction
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate)

出典と根拠

ORDレコード
ord-f1aa9cb6fca04ca9b6398103df5a9706
出典データセット
uspto-grants-2007_07
特許番号
US07244730B2

反応ノート

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