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

HRID 1280859노트

반응식

HRID 1280859 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
-15 °C

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-de03f40d19b84c4b9f564335b2fa3399
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06451858B2

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