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

HRID 35322

반응식

HRID 35322 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-377a94b0686f4107959ba1575d2f4d81
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766125

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