3-Amino-5-methyl-4H-1,2,4-triazole → HCID 178469337、化合物

HRID 973850

反応式

HRID 973850 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 178469337HCID 178469337、化合物収率 32.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5371e796ddc745a7aca9b7704cf9d928
出典データセット
uspto-grants-1991_11
特許番号
US05064953

関連ノート

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