Sulfuric Acid → 7-Methoxy-1-methyl-5-phenyl[1,2,4]triazolo[4,3-a]quinazoline

HRID 1414892ノート

反応式

HRID 1414892 の反応式
[NH:1]([C:3]1[N:12]=[C:11]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([O:19][CH3:20])[CH:9]=2)[N:4]=1)[NH2:2].[C:21]([O-])([O-])(OCC)[CH3:22].S(=O)(=O)(O)O>C(O)C>[CH3:21][C:22]1[N:4]2[C:5]3[C:10]([C:11]([C:13]4[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=4)=[N:12][C:3]2=[N:1][N:2]=1)=[CH:9][C:8]([O:19][CH3:20])=[CH:7][CH:6]=3

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 21485896HCID 21485896、化合物HCID 86598186Ethyl ortho-acetate

生成物 1

HCID 214859287-Methoxy-1-methyl-5-phenyl[1,2,4]triazolo[4,3-a]quinazoline

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In the next place, to a solution of 2.0 g of 2-hydrazino-4-phenyl-6-methoxyquinazoline in 100 ml of ethanol were added 3.5 g of ethyl orthoacetate and 0.5 ml of concentrated sulfuric acid. The resulting mixture was refluxed for 3 hours and then the solvent was removed under reduced pressure. To the residue was added ammonia water to basify, and the mixture was extracted with chloroform. The extract was washed with water, dried over anhydrous sodium sulfate and evaporated to dryness in vacuo. To the residue was added ethanol and the crystallized product was collected by filtration, and dried to give 1-methyl-5-phenyl-7-methoxy-s-triazolo[4,3-a]quinazoline as slightly yellow needles, m.p. 251° - 252° C.

後処理

  1. temperatureThe resulting mixture was refluxed for 3 hours
  2. customthe solvent was removed under reduced pressure
  3. additionTo the residue was added ammonia water
  4. extractionthe mixture was extracted with chloroform
  5. washThe extract was washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. customevaporated to dryness in vacuo
  8. additionTo the residue was added ethanol
  9. filtrationthe crystallized product was collected by filtration
  10. customdried

出典と根拠

ORDレコード
ord-074cbc054fa3473bb10d7cba46b99324
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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