Methyl Isocyanate → 4-Ethyl-5-(N-methyl-carbamoyl)-4,5,6,7-tetrahydro-imidazo-[4,5-c]-pyridine

HRID 1391220ノート

反応式

HRID 1391220 の反応式
[CH2:1]([CH:3]1[C:8]2[N:9]=[CH:10][NH:11][C:7]=2[CH2:6][CH2:5][NH:4]1)[CH3:2].[CH3:12][N:13]=[C:14]=[O:15]>O1CCOCC1.C(OCC)(=O)C>[CH2:1]([CH:3]1[C:8]2[N:9]=[CH:10][NH:11][C:7]=2[CH2:6][CH2:5][N:4]1[C:14](=[O:15])[NH:13][CH3:12])[CH3:2]

参加物

5

反応物 2

HCID 12228Methyl IsocyanateHCID 233422924-Ethyl-4,5,6,7-tetrahydro-3H-imidazo[4,5-c]pyridine

生成物 1

HCID 213307364-Ethyl-5-(N-methyl-carbamoyl)-4,5,6,7-tetrahydro-imidazo-[4,5-c]-pyridine

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

A solution of 1.51 g of 4-ethyl-4,5,6,7-tetrahydro-imidazo-[4,5-c]-pyridine and 2.28 g of methyl isocyanate in 20 ml of dry dioxane is refluxed for 1.5 h. The solution is cooled and filtered. The solid collected is dissolved in 30 ml of methanol and treated with 7 ml of 2N sodium hydroxide for 2 h at room temperature. After neutralization the solution is extracted with chloroform. Evaporation of the solvent leaves a residue that is taken up in ethyl acetate. 1.05 g of the title compound, m.p. 240°, are collected.

後処理

  1. temperatureThe solution is cooled
  2. filtrationfiltered
  3. customThe solid collected
  4. dissolutionis dissolved in 30 ml of methanol
  5. additiontreated with 7 ml of 2N sodium hydroxide for 2 h at room temperature
  6. extractionAfter neutralization the solution is extracted with chloroform
  7. customEvaporation of the solvent
  8. customleaves a residue that
  9. custom1.05 g of the title compound, m.p. 240°, are collected

出典と根拠

ORDレコード
ord-f5cfd79cde424ff9a634ee4cc70110bf
出典データセット
uspto-grants-1979_02
特許番号
US04141899

反応ノート

読み込み中…