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Chloroacetyl chloride → 2'-Bromo-5'-trifluoromethyl-2-chloroacetanilide

HRID 1464256
ノート
印刷プレビュー

反応式

HRID 1464256 の反応式
[Br:1][C:2]1[CH:8]=[CH:7][C:6]([C:9]([F:12])([F:11])[F:10])=[CH:5][C:3]=1[NH2:4].C(N(CC)CC)C.[Cl:20][CH2:21][C:22](Cl)=[O:23]>C(Cl)Cl>[Br:1][C:2]1[CH:8]=[CH:7][C:6]([C:9]([F:10])([F:11])[F:12])=[CH:5][C:3]=1[NH:4][C:22](=[O:23])[CH2:21][Cl:20]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6577Chloroacetyl chlorideHCID 8471TriethylamineHCID 679892-Bromo-5-(trifluoromethyl)benzenamine

生成物 1

HCID 157139482'-Bromo-5'-trifluoromethyl-2-chloroacetanilide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To a solution of 2-bromo-5-trifluoromethylaniline (10.0 g) in methylene chloride (100 ml) was added triethylamine and the solution was cooled to 0° C. To this solution was slowly added choroacetyl chloride and the reaction mixture was allowed to cool to room temperature overnight. The solution was concentrated and the resulting solid was extracted with ethyl acetate. The organic extract was first washed with 10% HCl (2×2 ml), then with water (12×25 ml) and was collected, dried and evaporated to obtain the title compound (yield, 10.2 g). 1HNMR (250 MHz, CDCl3): 4.22 (s, 2 H), 7.26 (d, J=8 Hz, 1 H), 7.66 (d, J=8 Hz, 1 Hz), 8.68 (s, 1 H), 9.02 (br s, 1 H).

後処理

  1. temperatureto cool to room temperature overnight
  2. concentrationThe solution was concentrated
  3. extractionthe resulting solid was extracted with ethyl acetate
  4. extractionThe organic extract
  5. washwas first washed with 10% HCl (2×2 ml)
  6. customwith water (12×25 ml) and was collected
  7. customdried
  8. customevaporated

出典と根拠

ORDレコード
ord-c8665eba631f41fd986e3dd0e0027af3
出典データセット
uspto-grants-1994_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05304557

反応ノート

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