Water → 2,6-dichloro-N-(2-chloroethyl)benzamide

HRID 345534

반응식

HRID 345534 반응식
Cl.[Cl:2][CH2:3][CH2:4][NH2:5].C(=O)([O-])[O-].[K+].[K+].O.[Cl:13][C:14]1[CH:22]=[CH:21][CH:20]=[C:19]([Cl:23])[C:15]=1[C:16](Cl)=[O:17]>ClCCl>[Cl:13][C:14]1[CH:22]=[CH:21][CH:20]=[C:19]([Cl:23])[C:15]=1[C:16]([NH:5][CH2:4][CH2:3][Cl:2])=[O:17]

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 783922,6-Dichlorobenzoyl chlorideHCID 97937372-Chloroethylamine hydrochloride

생성물 1

HCID 150969722,6-dichloro-N-(2-chloroethyl)benzamide수율 68.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred (vigorously) mixture of 17.4 parts of 2-chloroethanamine hydrochloride, 20.7 parts of potassium carbonate and 225 parts of water was added dropwise a mixture of 31.3 parts of 2,6-dichlorobenzoyl chloride and 120 parts of dichloromethane at room temperature: slightly exothermic reaction. Upon completion, stirring at room temperature was continued for one hour. The organic phase was separated and the aqueous phase was extracted with dichloromethane. The combined organic phases were washed with water, dried, filtered and evaporated. The residue was crystallized from methylbenzene. The product was filtered off and dried, yielding 25.8 parts (68.8%) of 2,6-dichloro-N-(2-chloroethyl)benzamide; mp. 113.8° C. (intermediate 30).

후처리

  1. additionwas added dropwise
  2. customslightly exothermic reaction
  3. stirringUpon completion, stirring at room temperature
  4. customThe organic phase was separated
  5. extractionthe aqueous phase was extracted with dichloromethane
  6. washThe combined organic phases were washed with water
  7. customdried
  8. filtrationfiltered
  9. customevaporated
  10. customThe residue was crystallized from methylbenzene
  11. filtrationThe product was filtered off
  12. customdried

출처 및 근거

ORD 기록
ord-73df445bc2dd411ba963a40e2193eb22
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05057525

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