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

HRID 1290812노트

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HRID 1290812 반응식
[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]

참가 물질

4

반응물 2

HCID 4362726HCID 4362726, 화합물HCID 178418311HCID 178418311, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

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.).

후처리

  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.)

출처 및 근거

ORD 기록
ord-4f36e255efb64a5483ec38ca23ccfbd9
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753665

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