Chloroacetyl chloride → 2-chloro-N-(2-chloro-6-fluorophenyl)-N-(4-methylphenyl)acetamide

HRID 1242256

反応式

HRID 1242256 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[NH:9][C:10]1[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][CH:11]=1.[Cl:17][CH2:18][C:19](Cl)=[O:20].CCCCC>C(OCC)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[N:9]([C:19](=[O:20])[CH2:18][Cl:17])[C:10]1[CH:11]=[CH:12][C:13]([CH3:16])=[CH:14][CH:15]=1

参加物

5

反応物 3

HCID 6577Chloroacetyl chlorideHCID 8003PentaneHCID 21100364(2-Chloro-6-fluorophenyl)-P-tolyl-amine

生成物 1

HCID 46729202-chloro-N-(2-chloro-6-fluorophenyl)-N-(4-methylphenyl)acetamide

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
-15 °C

実験手順

A mixture of 25 g (0.11 mol) N-(2′-chloro-6′-fluorophenyl)-4-methylaniline and 40 ml (0.5 mol) of chloroacetylchloride is heated under a nitrogen atmosphere for 15 minutes at 60°. The solvent is evaporated under reduced pressure to give an oil which is dissolved in 25 ml of ethyl acetate. Pentane (250 ml) is added dropwise over 15 minutes to precipitate the product. The mixture is cooled to −15° C. and the solid is filtered and washed with pentane to give N-(2′-chloro-6′-fluorophenyl)-N-chloroacetyl-4-methylaniline, m.p. 80–83°.

後処理

  1. temperatureis heated under a nitrogen atmosphere for 15 minutes at 60°
  2. customThe solvent is evaporated under reduced pressure
  3. customto give an oil which
  4. customto precipitate the product
  5. filtrationthe solid is filtered
  6. washwashed with pentane

出典と根拠

ORDレコード
ord-94074bad72a84be8b1d96a8a12ba9b93
出典データセット
uspto-grants-2006_10
特許番号
US07115662B2

関連ノート

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