Ammonium Chloride → HCID 68320915、化合物

HRID 2047467ノート

反応式

HRID 2047467 の反応式
Cl.[CH3:2][C:3]1[CH:4]=[C:5]([CH:7]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:9]=1)[NH2:6].[C:14](Cl)(=[O:25])[O:15][C:16]1[CH:21]=[CH:20][C:19]([N+:22]([O-:24])=[O:23])=[CH:18][CH:17]=1.C(N(CC)C(C)C)(C)C.[Cl-].[NH4+]>C1COCC1>[CH3:2][C:3]1[CH:4]=[C:5]([NH:6][C:14](=[O:25])[O:15][C:16]2[CH:17]=[CH:18][C:19]([N+:22]([O-:24])=[O:23])=[CH:20][CH:21]=2)[CH:7]=[C:8]([C:10]([F:11])([F:12])[F:13])[CH:9]=1

参加物

6

反応物 4

HCID 25517Ammonium ChlorideHCID 81531DiisopropylethylamineHCID 821294-Nitrophenyl chloroformateHCID 866556663-Methyl-5-(trifluoromethyl)aniline hydrochloride

生成物 1

HCID 68320915HCID 68320915、化合物収率 98.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
5 °C

実験手順

3-Methyl-5-(trifluoromethyl)aniline monohydrochloride (2.93 g) synthesized in reference to a known method (U.S. Pat. No. 4,532,353) was dissolved in THF (25 mL), and 4-nitrophenyl chlorocarbonate (3.07 g) and N,N-diisopropylethylamine (1.97 mL) were added dropwise at 5° C. The reaction mixture was stirred at 5° C. for 1 hr, poured into saturated aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, dried and concentrated under reduced pressure to give the title compound (4.66 g) as a white powder.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with water and saturated brine
  3. customdried
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-567a16b07d4f48649a629d309bec7986
出典データセット
uspto-grants-2013_11
特許番号
US08592454B2

反応ノート

読み込み中…