Hydrochloric Acid → 4-Hexyl-1,2,4-triazolidine-3,5-dione

HRID 2296384

反応式

HRID 2296384 の反応式
[C:1]([NH:4][NH:5][C:6]([NH2:8])=[O:7])(N)=[O:2].[CH2:9](N)[CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].Cl>CN1CCCC1=O>[CH2:9]([N:8]1[C:6](=[O:7])[NH:5][NH:4][C:1]1=[O:2])[CH2:10][CH2:11][CH2:12][CH2:13][CH3:14]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 80391,2-HydrazinedicarboxamideHCID 8102Hexylamine

生成物 1

HCID 204701154-Hexyl-1,2,4-triazolidine-3,5-dione

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

60 g of hydrazodicarbonamide and 56 g of n-hexylamine are stirred in 100 ml of N-methy pyrrolidone for 6 hours at 150° C., for 20 hours at 175° C. and for 20 hours at 180° C. The solvent is then distilled off in vacuo and the residue is triturated with 100 ml of 10% sodium hydroxide solution. The deposit is isolated by filtration under suction and the filtrate is neutralised with 10% hydrochloric acid. A deposit is precipitated and is isolated by filtration under suction, washed with water and dried in vacuo, giving 75 g (81% of the theoretical yield) of 4-(n-hexyl)-1,2,4-triazolidine-3,5-dione in the form of colourless crystals melting at 144° C. to 145° C.

後処理

  1. distillationThe solvent is then distilled off in vacuo
  2. customthe residue is triturated with 100 ml of 10% sodium hydroxide solution
  3. customThe deposit is isolated by filtration under suction
  4. customA deposit is precipitated
  5. customis isolated by filtration under suction
  6. washwashed with water
  7. customdried in vacuo
  8. customgiving 75 g (81% of the

出典と根拠

ORDレコード
ord-e983ca716a2840219f9398b2e6ee80f2
出典データセット
uspto-grants-1984_01
特許番号
US04429135

関連ノート

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