Dimethylcarbamoyl Chloride → 1-(N,N-Dimethylcarbamoyl)-4,5-dicyanoimidazole

HRID 27032

反応式

HRID 27032 の反応式
O1CCOCC1.[C:7]([C:9]1[N:10]=[CH:11][NH:12][C:13]=1[C:14]#[N:15])#[N:8].C(N(CC)CC)C.[CH3:23][N:24]([CH3:28])[C:25](Cl)=[O:26]>>[CH3:23][N:24]([CH3:28])[C:25]([N:10]1[C:9]([C:7]#[N:8])=[C:13]([C:14]#[N:15])[N:12]=[CH:11]1)=[O:26]

参加物

5

反応物 4

HCID 6598Dimethylcarbamoyl ChlorideHCID 8471TriethylamineHCID 312751,4-DioxaneHCID 707294,5-Dicyanoimidazole

生成物 1

HCID 233434181-(N,N-Dimethylcarbamoyl)-4,5-dicyanoimidazole

実験手順

To 50 ml of dry 1,4-dioxane 6.0 g (0.05 mole) of 4,5-dicyanoimidazole, 5.0 g (0.05 mole) of triethylamine and 6.0 g (0.055 mole) of dimethylcarbamoyl chloride are added in succession at room temperature. This mixture is stirred and refluxed for 3 days, cooled to room temperature and evaporated to dryness. The residue is stirred in 50 ml of ethyl acetate and 50 ml water. The organic layer is separated, washed, dried and evaporated to give 8 g. (85%) of white product.

後処理

  1. temperaturerefluxed for 3 days
  2. customevaporated to dryness
  3. stirringThe residue is stirred in 50 ml of ethyl acetate
  4. customThe organic layer is separated
  5. washwashed
  6. customdried
  7. customevaporated
  8. customto give 8 g

出典と根拠

ORDレコード
ord-ccbdcc529e104ca9a8cdaf4b5e1e4621
出典データセット
uspto-grants-1980_09
特許番号
US04220466

関連ノート

読み込み中…