3-(Trifluoromethyl)aniline → 8-ethyl-2-methyl-N-[3-(trifluoromethyl)-phenyl]-8H-pyrazolo[1,5-a]pyrazolo[4',3':5,6]pyrido[3,4-e]-pyrimidin-5-amine

HRID 1395222노트

반응식

HRID 1395222 반응식
Cl[C:2]1[C:7]2[CH:8]=[N:9][C:10]3[N:14]([CH2:15][CH3:16])[N:13]=[CH:12][C:11]=3[C:6]=2[N:5]2[N:17]=[C:18]([CH3:20])[CH:19]=[C:4]2[N:3]=1.C(N(CC)CC)C.[F:28][C:29]([F:38])([F:37])[C:30]1[CH:31]=[C:32]([CH:34]=[CH:35][CH:36]=1)[NH2:33]>C(O)CCC>[CH2:15]([N:14]1[C:10]2[N:9]=[CH:8][C:7]3[C:2]([NH:33][C:32]4[CH:34]=[CH:35][CH:36]=[C:30]([C:29]([F:28])([F:37])[F:38])[CH:31]=4)=[N:3][C:4]4[N:5]([N:17]=[C:18]([CH3:20])[CH:19]=4)[C:6]=3[C:11]=2[CH:12]=[N:13]1)[CH3:16]

참가 물질

5

반응물 3

HCID 73753-(Trifluoromethyl)anilineHCID 8471TriethylamineHCID 537035595-chloro-8-ethyl-2-methyl-8H-pyrazolo[1,5-a]pyrazolo[4',3':5,6]pyrido[3,4-e]pyrimidine

생성물 1

HCID 233316038-ethyl-2-methyl-N-[3-(trifluoromethyl)-phenyl]-8H-pyrazolo[1,5-a]pyrazolo[4',3':5,6]pyrido[3,4-e]-pyrimidin-5-amine수율 72.9%

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

5.8 g of 5-chloro-8-ethyl-2-methyl-8H-pyrazolo[1,5-a]pyrazolo[4',3':5,6]pyrido[3,4-e]pyrimidine (0.02 mol), 3 g of triethylamine and 3.3 g of 3-trifluoromethylaniline are refluxed in butyl alcohol for 24 hours with stirring. The solvent is removed in vacuo and the residue treated with 20 ml of water and filtered off. Recrystallization from alcohol yields 6 g of 8-ethyl-2-methyl-N-[3-(trifluoromethyl)phenyl]-8H-pyrazolo[1,5-a]pyrazolo[4',3':5,6]pyrido[3,4-e]pyrimidin-5-amine; yield (73%) m.p. 205°-206°.

후처리

  1. customThe solvent is removed in vacuo
  2. additionthe residue treated with 20 ml of water
  3. filtrationfiltered off
  4. customRecrystallization from alcohol

출처 및 근거

ORD 기록
ord-d441c523c4634a499cd7ee1ce41fd21d
출처 데이터셋
uspto-grants-1980_05
특허 번호
US04202899

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