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

HRID 2296385

반응식

HRID 2296385 반응식
[CH2:1]([NH2:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:9]([NH:12][NH:13][C:14](N)=[O:15])(N)=[O:10].Cl>CN1CCCC1=O>[CH2:1]([N:8]1[C:14](=[O:15])[NH:13][NH:12][C:9]1=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 7504BenzylamineHCID 80391,2-Hydrazinedicarboxamide

생성물 1

HCID 3923314-Benzyl-1,2,4-triazolidine-3,5-dione

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

53.5 g of benzylamine and 59 g of hydrazodicarbonamide are stirred in 100 ml of N-methyl pyrrolidone for 4 hours at 175° C. and for 5 hours at 200° C. The solvent is then distilled off in vacuo, the residue is triturated with 50 ml of a 10% sodium hydroxide solution and the residue is isolated by filtration under suction. The filtrate is neutralised with 10% hydrochloric acid. A deposit is formed which is filtered off under suction and washed with water, giving 67 g (70% of the theoretical yield) of 4-benzyl-1,2,4-triazolidine-3,5-dione in the form of colourless crystals melting at 185° to 188° C. (CH3CN).

후처리

  1. distillationThe solvent is then distilled off in vacuo
  2. customthe residue is triturated with 50 ml of a 10% sodium hydroxide solution
  3. customthe residue is isolated by filtration under suction
  4. customA deposit is formed which
  5. filtrationis filtered off under suction
  6. washwashed with water
  7. customgiving 67 g (70% of the

출처 및 근거

ORD 기록
ord-499190fca63640a4a4c48a8c49984930
출처 데이터셋
uspto-grants-1984_01
특허 번호
US04429135

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