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

HRID 1414896노트

반응식

HRID 1414896 반응식
[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

참가 물질

5

반응물 2

HCID 222AmmoniaHCID 12246017HCID 12246017, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f8f3a259f30945d793bd79cc3c95e98d
출처 데이터셋
uspto-grants-1977_01
특허 번호
US04002755

반응 노트

불러오는 중…