Cyanuric chloride → 4,6-dichloro-2-ethoxycarbonylmethylamino-S-triazine

HRID 1757606

反応式

HRID 1757606 の反応式
[N:1]1[C:8]([Cl:9])=[N:7][C:5](Cl)=[N:4][C:2]=1[Cl:3].Cl.[NH2:11][CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14].C(=O)(O)[O-].[Na+]>>[Cl:9][C:8]1[N:1]=[C:2]([Cl:3])[N:4]=[C:5]([NH:11][CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])[N:7]=1

参加物

4

反応物 3

HCID 7954Cyanuric chlorideHCID 516892Sodium BicarbonateHCID 2723640Glycine ethyl ester, hydrochloride

生成物 1

HCID 147462614,6-dichloro-2-ethoxycarbonylmethylamino-S-triazine

実験手順

36.9 g of cyanuric chloride, 27.9 g of ethyl glycinate hydrochloride and 33.6 g of sodium bicarbonate were heated under reflux in 200 ml of dioxanefor 30 minutes. At the end of this time, the dioxane was removed by distillation under reduced pressure, and a mixture of ethyl acetate and water was added to the resulting residue, after which the mixture was shaken. The ethyl acetate layer was separated, dried and concentrated by evaporation under reduced pressure, and the resulting residue was recrystallized from a mixture of hexane and ethyl acetate, to yield 45.0 gof the title compound as crystals melting at 82° to 87° C.

後処理

  1. temperatureunder reflux in 200 ml of dioxanefor 30 minutes
  2. customAt the end of this time, the dioxane was removed by distillation under reduced pressure
  3. additiona mixture of ethyl acetate and water
  4. additionwas added to the resulting residue
  5. customThe ethyl acetate layer was separated
  6. customdried
  7. concentrationconcentrated by evaporation under reduced pressure
  8. customthe resulting residue was recrystallized from a mixture of hexane and ethyl acetate

出典と根拠

ORDレコード
ord-a263c55c9326424cab865273cb512687
出典データセット
uspto-grants-1995_08
特許番号
US05446144

関連ノート

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