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 224619ノート

反応式

HRID 224619 の反応式
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]

参加物

5

反応物 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

生成物 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-amine収率 72.9%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

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°.

後処理

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

出典と根拠

ORDレコード
ord-28dac4fc4fb74a3bb911951becc08582
出典データセット
uspto-grants-1980_11
特許番号
US04233300

反応ノート

読み込み中…