Toluene → 2-Chloro-2'-methoxy-5'-methylacetanilide

HRID 35323

반응식

HRID 35323 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH3:9])=[CH:5][C:4]=1[NH2:10].CC1C=CC=CC=1.[Cl:18][CH2:19][C:20](Cl)=[O:21]>O>[Cl:18][CH2:19][C:20]([NH:10][C:4]1[CH:5]=[C:6]([CH3:9])[CH:7]=[CH:8][C:3]=1[O:2][CH3:1])=[O:21]

참가 물질

5

반응물 3

HCID 1140TolueneHCID 6577Chloroacetyl chlorideHCID 84452-Methoxy-5-Methylaniline

생성물 1

HCID 7369912-Chloro-2'-methoxy-5'-methylacetanilide수율 66%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred solution of 49.2 parts of 2-methoxy-5-methylbenzenamine and 270 parts of methylbenzene were added dropwise 22.5 parts of 2-chloroacetyl chloride while cooling (ice-bath) at 10°-20° C. Upon completion, stirring was continued for 1.50 hours at room temperature. 200 Parts of water were added. The organic phase was separated, washed with water, dried, filtered and evaporated. The oily residue was crystallized from 2,2'-oxybispropane. The product was filtered off and dried, yielding 28.2 parts (66%) of 2-chloro-N-(2-methoxy-5-methylphenyl)acetamide; mp. 83.9° C. (intermediate 66).

후처리

  1. temperaturewhile cooling (ice-bath) at 10°-20° C
  2. customThe organic phase was separated
  3. washwashed with water
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. customThe oily residue was crystallized from 2,2'-oxybispropane
  8. filtrationThe product was filtered off
  9. customdried

출처 및 근거

ORD 기록
ord-fc76ba613db148e5b72e5a3ba33e1cb9
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766125

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