Pyridine → 1,3,5-Benzenetricarbonitrile, 2,4,6-trimethyl-

HRID 855472ノート

反応式

HRID 855472 の反応式
[C:1]([Cu])#[N:2].[N:4]1[CH:9]=CC=CC=1.Br[C:11]1[C:16]([CH3:17])=[C:15](Br)[C:14]([CH3:19])=[C:13](Br)[C:12]=1[CH3:21].[CH2:22](N)[NH2:23]>>[C:22]([C:11]1[C:16]([CH3:17])=[C:15]([C:9]#[N:4])[C:14]([CH3:19])=[C:13]([C:1]#[N:2])[C:12]=1[CH3:21])#[N:23]

参加物

5

反応物 4

HCID 1049PyridineHCID 75408MethanediamineHCID 2629821,3,5-tribromo-2,4,6-trimethylbenzeneHCID 178418546HCID 178418546、化合物

生成物 1

HCID 1210551,3,5-Benzenetricarbonitrile, 2,4,6-trimethyl-

実験手順

CuCN (220 g, 243 mmol) and pyridine (146.7 g, 1.85 mol) were added to a high pressure reaction vessel, and well mixed, and then 2,4,6-tribromo-1,3,5-trimethylbenzene(25 g, 75.8 mmol) was added thereto. The reaction mixture was reacted at 205° C. for 2 hours. Cu therein was excluded with excessive methylene diamine, and then filtered by MC. Water in the reaction mixture was eliminated over MgSO4, and then solvent therein was evaporated in vacuum. The residue was absorbed to silica gel column and separated with a tube chromatography (Hx:MC=3:1) to obtain white solid [yield : 6 g (40.59%)].

後処理

  1. additionwell mixed
  2. customThe reaction mixture was reacted at 205° C. for 2 hours
  3. filtrationfiltered by MC
  4. customsolvent therein was evaporated in vacuum
  5. customThe residue was absorbed to silica gel column
  6. customseparated with a tube chromatography (Hx:MC=3:1)
  7. customto obtain white solid [yield : 6 g (40.59%)]

出典と根拠

ORDレコード
ord-9586d76a007b444bb8c2bafbcc20e156
出典データセット
uspto-grants-2007_08
特許番号
US07261952B2

反応ノート

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