Acetonitrile → HCID 135611167、化合物

HRID 1015422ノート

反応式

HRID 1015422 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([C:14]([F:17])([F:16])[F:15])=[CH:10][CH:9]=2)=[CH:4][C:3]=1[C:18]1[NH:22][C:21](=[O:23])[O:20][N:19]=1.[F:24][C:25]1[CH:26]=[C:27]([N:32]=[C:33]=[O:34])[CH:28]=[C:29]([F:31])[CH:30]=1.C(#N)C>C1(C)C=CC=CC=1>[F:24][C:25]1[CH:26]=[C:27]([NH:32][C:33]([NH:1][C:2]2[CH:7]=[CH:6][C:5]([C:8]3[CH:9]=[CH:10][C:11]([C:14]([F:15])([F:16])[F:17])=[CH:12][CH:13]=3)=[CH:4][C:3]=2[C:18]2[NH:22][C:21](=[O:23])[O:20][N:19]=2)=[O:34])[CH:28]=[C:29]([F:31])[CH:30]=1

参加物

5

反応物 3

HCID 6342AcetonitrileHCID 27792821,3-Difluoro-5-isocyanatobenzene3 回HCID 136075215HCID 136075215、化合物

生成物 1

HCID 135611167HCID 135611167、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

In 100 ml of dry toluene was 5 g of 3-(4-amino-4′-trifluoromethyl-biphenyl-3-yl)-4H-[1,2,4]oxadiazol-5-one suspended and 2.5 g of 3,5-difluorophenyl isocyanate was added, the reaction mixture was stirred at room temperature overnight, 1.3 g of 3,5-difluorophenyl isocyanate was added and stirring was continued overnight. 3,5-Difluorophenyl isocyanate (1.3 g) and 100 ml of acetonitrile was added, the reaction mixture was stirred at room temperature for 90 min. and evaporated to dryness. The residue was dissolved in 100 ml of boiling acetone, then cooled to 0° C. and filtrated. The precipitate was recrystallized from 200 ml of ethanol, after filtration while hot, the solution was added 400 ml of water. The product was isolated by filtration. Yield 4 g (54%) mp.>150° C. decomp.

後処理

  1. stirringstirring
  2. waitwas continued overnight
  3. stirringthe reaction mixture was stirred at room temperature for 90 min.
  4. customevaporated to dryness
  5. dissolutionThe residue was dissolved in 100 ml of boiling acetone
  6. temperaturecooled to 0° C.
  7. filtrationfiltrated
  8. customThe precipitate was recrystallized from 200 ml of ethanol
  9. filtrationafter filtration while hot, the solution
  10. additionwas added 400 ml of water
  11. customThe product was isolated by filtration

出典と根拠

ORDレコード
ord-ea4b952fa442446cb9da3fcd38140bcf
出典データセット
uspto-grants-2011_07
特許番号
US07985761B2

反応ノート

読み込み中…