Ammonia → [1,2,4]Triazolo[4,3-a]quinazoline, 7-chloro-1-methyl-5-phenyl-

HRID 1414896ノート

反応式

HRID 1414896 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:16]2[C:20](Br)=[N:19][N:18]=[C:17]2[CH3:22])=[C:6]([CH:15]=1)[C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=O.[NH3:23]>CS(C)=O.C(Cl)(Cl)Cl>[CH3:22][C:17]1[N:16]2[C:5]3[C:6]([C:7]([C:9]4[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=4)=[N:23][C:20]2=[N:19][N:18]=1)=[CH:15][C:2]([Cl:1])=[CH:3][CH:4]=3

参加物

5

反応物 2

HCID 222AmmoniaHCID 12246017HCID 12246017、化合物

生成物 1

HCID 1869146[1,2,4]Triazolo[4,3-a]quinazoline, 7-chloro-1-methyl-5-phenyl-

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 6212Chloroform溶媒

実験手順

In the next place, a solution of 0.5 g of the above-mentioned 5-chloro-2-(3-methyl-5-bromo-4H-1,2,4-triazol-4-yl)benzophenone in 20 ml of dimethylsulfoxide was heated, with stirring, at about 180° C for 10 hours, during which ammonia gas was continuously passed into the reaction mixture. After cooling, the reaction mixture was poured into ice-water and the resulting crystals were filtered, washed with water and dried. The crystals thus obtained was dissolved in chloroform and chromatographed on silica gel using chloroform as an eluent. The product thus separated was recrystallized from isopropyl ether to give 1-methyl-5-phenyl-7-chloro-s-triazolo[4,3-a]quinazoline, m.p. 325° - 327° C.

後処理

  1. temperatureAfter cooling
  2. filtrationthe resulting crystals were filtered
  3. washwashed with water
  4. customdried
  5. customThe crystals thus obtained
  6. customchromatographed on silica gel
  7. customThe product thus separated
  8. customwas recrystallized from isopropyl ether

出典と根拠

ORDレコード
ord-f8f3a259f30945d793bd79cc3c95e98d
出典データセット
uspto-grants-1977_01
特許番号
US04002755

反応ノート

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