Acetic Acid → 2-chloro-N-[2-methoxy-5-(trifluoromethyl)phenyl]-acetamide

HRID 35322

反応式

HRID 35322 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([F:12])([F:11])[F:10])=[CH:5][C:4]=1[NH2:13].C(O)(=O)C.[Cl:18][CH2:19][C:20](Cl)=[O:21].C([O-])(=O)C.[Na+]>O>[Cl:18][CH2:19][C:20]([NH:13][C:4]1[CH:5]=[C:6]([C:9]([F:11])([F:10])[F:12])[CH:7]=[CH:8][C:3]=1[O:2][CH3:1])=[O:21]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 6577Chloroacetyl chlorideHCID 517045Sodium AcetateHCID 6006372-Methoxy-5-(trifluoromethyl)aniline

生成物 1

HCID 142302752-chloro-N-[2-methoxy-5-(trifluoromethyl)phenyl]-acetamide収率 93.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a stirred and cooled (about 10° C.) solution of 11.7 parts of 2-methoxy-5-(trifluoromethyl)benzenamine in 50 parts of acetic acid were added dropwise 7.7 parts of chloroacetyl chloride at a temperature below 20° C. After stirring for 30 minutes, there was added dropwise a solution of 24.8 parts of sodium acetate in 62 parts of water (exothermic reaction). Upon completion, stirring was continued for 30 minutes at room temperature. The precipitated product was filtered off, washed with a lot of water and dried, yielding 15.5 parts (93.3%) of 2-chloro-N-[2-methoxy-5-(trifluoromethyl)phenyl]-acetamide; mp. 94.7° C. (intermediate 62).

後処理

  1. stirringAfter stirring for 30 minutes
  2. stirringUpon completion, stirring
  3. filtrationThe precipitated product was filtered off
  4. washwashed with a lot of water
  5. customdried

出典と根拠

ORDレコード
ord-377a94b0686f4107959ba1575d2f4d81
出典データセット
uspto-grants-1988_08
特許番号
US04766125

関連ノート

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