Benzylamine → 4-Benzyl-1,2,4-triazolidine-3,5-dione

HRID 1388757

反応式

HRID 1388757 の反応式
[CH2:1]([NH2:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH:9]([C:14](N)=[O:15])[NH:10][C:11](N)=[O:12]>CN1CCCC1=O>[CH2:1]([N:8]1[C:11](=[O:12])[NH:10][NH:9][C:14]1=[O:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 7504BenzylamineHCID 80391,2-Hydrazinedicarboxamide

生成物 1

HCID 3923314-Benzyl-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

53.5 g of benzylamine and 59 g of hydrazodicarboxamide in 100 ml of N-methylpyrrolidone are stirred at 175° C. for 4 hours and at 200° C. for 5 hours. The solvent is then distilled off in vacuo, the residue is triturated with 50 ml of 10% strength sodium hydroxide solution, and the resulting residue is filtered off. The filtrate is neutralised with 10% strength hydrochloric acid. A precipitate is thereby formed and is filtered off and washed with water. 67 g (70% of the theoretical yield) of 4-benzyl-1,2,4-triazolidine-3,5-dione are obtained as colourless cyrstals of melting point 185°-188° C. (CH3CN).

後処理

  1. distillationThe solvent is then distilled off in vacuo
  2. customthe residue is triturated with 50 ml of 10% strength sodium hydroxide solution
  3. filtrationthe resulting residue is filtered off
  4. customA precipitate is thereby formed
  5. filtrationis filtered off
  6. washwashed with water

出典と根拠

ORDレコード
ord-4cc51fc194294dbd93346c48a1e242d4
出典データセット
uspto-grants-1984_02
特許番号
US04433085

関連ノート

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