3-Methyl-2,4-pentanedione → 2-Benzylsulfanyl-5,6,7-trimethyl-[1,2,4]triazolo[1,5-a]pyrimidine

HRID 844958

反応式

HRID 844958 の反応式
[NH2:1][C:2]1[N:6]=[C:5]([S:7][CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[NH:4][N:3]=1.[CH3:15][CH:16]([C:20](=O)[CH3:21])[C:17](=O)[CH3:18]>C(O)(=O)C>[CH2:8]([S:7][C:5]1[N:6]=[C:2]2[N:1]=[C:17]([CH3:18])[C:16]([CH3:15])=[C:20]([CH3:21])[N:3]2[N:4]=1)[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

参加物

4

反応物 2

HCID 699493-Methyl-2,4-pentanedioneHCID 178509291HCID 178509291、化合物

生成物 1

HCID 6250072-Benzylsulfanyl-5,6,7-trimethyl-[1,2,4]triazolo[1,5-a]pyrimidine収率 94.4%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 51.6 g (0.250 mol) of 3-amino-5-benzylthio-1,2,4-triazole and 28.5 g (0.250 mol) of 3-methyl-2,4-pentanedione in 350 ml of glacial acetic acid was heated at reflux for 17 hours. Upon cooling to room temperature, the reaction mixture was poured onto ice. The pale yellow solid which separated was collected by filtration, washed with water and dried in vacuo to yield 67.1 g (94%) of the desired product as a pale yellow solid, m.p. 133.5°-135° C. The IR and 1H NMR spectra were consistent with the assigned structure.

後処理

  1. temperatureat reflux for 17 hours
  2. additionthe reaction mixture was poured onto ice
  3. customThe pale yellow solid which separated
  4. filtrationwas collected by filtration
  5. washwashed with water
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-2b24c8f3d42343d8b7b252a1f9c97701
出典データセット
uspto-grants-1988_07
特許番号
US04755212

関連ノート

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