3-Amino-5-methyl-4H-1,2,4-triazole → HCID 178469337, 화합물

HRID 477545

반응식

HRID 477545 반응식
[NH2:1][C:2]1[N:6]=[C:5]([CH3:7])[NH:4][N:3]=1.[C:8]([C:13]([O:15][CH2:16][CH3:17])=[O:14])#[C:9][C:10]([O-])=[O:11]>C(O)C>[CH2:16]([O:15][C:13]([C:8]1[CH:9]=[C:10]([OH:11])[N:6]2[C:5]([CH3:7])=[N:4][N:3]=[C:2]2[N:1]=1)=[O:14])[CH3:17]

참가 물질

4

반응물 2

HCID 2346103-Amino-5-methyl-4H-1,2,4-triazoleHCID 713605752-Butynedioic acid, monoethyl ester

생성물 1

HCID 178469337HCID 178469337, 화합물수율 32.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A suspension of 14.7 g of 3-amino-5-methyl-s-triazole and 26.8 g of ethyl acetylenedicarboxylate in 120 ml of ethanol was refluxed for three hours, the reaction mixture was allowed to stand at room temperature for one hour, and the formed crystals were collected by filtration. The filtrate was concentrated and the residue was recrystallized from dichloromethane, and the crystals were joined with those obtained above. Purification by silica gel chromatography gave 10.8 g of the objective compound as colorless crystals.

후처리

  1. temperaturewas refluxed for three hours
  2. filtrationthe formed crystals were collected by filtration
  3. concentrationThe filtrate was concentrated
  4. customthe residue was recrystallized from dichloromethane
  5. customthose obtained above
  6. customPurification by silica gel chromatography

출처 및 근거

ORD 기록
ord-f2a342a9eb6b4a2bbadb50739037fd98
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04888332

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