HCID 4362726、化合物 → 7-[1-(2,4-Dichlorophenoxy)ethyl]-[1,2,4]triazolo[1,5-a]pyrimidine

HRID 1290812ノート

反応式

HRID 1290812 の反応式
[Cl:1][C:2]1[CH:17]=[C:16]([Cl:18])[CH:15]=[CH:14][C:3]=1[O:4][CH:5]([CH3:13])[C:6](=O)[CH:7]=[CH:8][N:9](C)[CH3:10].[NH2:19][C:20]1N=C[NH:22][N:21]=1>C(O)(=O)C>[Cl:1][C:2]1[CH:17]=[C:16]([Cl:18])[CH:15]=[CH:14][C:3]=1[O:4][CH:5]([C:6]1[N:22]2[N:21]=[CH:20][N:19]=[C:10]2[N:9]=[CH:8][CH:7]=1)[CH3:13]

参加物

4

反応物 2

HCID 4362726HCID 4362726、化合物HCID 178418311HCID 178418311、化合物

生成物 1

HCID 38014747-[1-(2,4-Dichlorophenoxy)ethyl]-[1,2,4]triazolo[1,5-a]pyrimidine

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

A solution of 4-(2,4-dichlorophenoxy)-1-(dimethylamino)-1-penten-3-one (2.9 g) in glacial acetic acid (25 ml) was added to a stirred solution of 3-amino-1,2,4-triazole (0.93 g) also in glacial acetic acid (25 ml). The mixture was heated under reflux for 5 hours and then cooled to room temperature. The mixture was then poured into 200 ml of ice-water and extracted with toluene. The toluene extracts were washed with a 10% aqueous solution of sodium hydrogen carbonate followed by water, then dried over anhydrous magnesium sulphate and the solvent was evaporated under reduced pressure. The residue was triturated with cold diethyl ether and the solid was collected by filtration, followed by recrystallisation from a mixture of ethyl acetate and petroleum ether (b.p. 40°-60° C.) to give 7-[1-(2,4-dichlorophenoxy)ethyl]-1,2,4-triazolo[1,5-a]pyrimidine. Yield 2.02 g, (mp 137°-138° C.).

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 5 hours
  3. extractionextracted with toluene
  4. washThe toluene extracts were washed with a 10% aqueous solution of sodium hydrogen carbonate
  5. dry with materialdried over anhydrous magnesium sulphate
  6. customthe solvent was evaporated under reduced pressure
  7. customThe residue was triturated with cold diethyl ether
  8. filtrationthe solid was collected by filtration
  9. customfollowed by recrystallisation from a mixture of ethyl acetate and petroleum ether (b.p. 40°-60° C.)

出典と根拠

ORDレコード
ord-4f36e255efb64a5483ec38ca23ccfbd9
出典データセット
uspto-grants-1998_05
特許番号
US05753665

反応ノート

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