Chloroacetyl chloride → N-(2',6'-dichlorophenyl)-N-chloroacetyl-4-methylaniline

HRID 603348

반응식

HRID 603348 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl: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]>>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl: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

3

실험 절차

N-(2′,6′-Dichlorophenyl)-4-methylaniline (4.86 g) is reacted with chloroacetylchloride (3.92 g) at 90° C. for 2 h. After dilution with toluene, the mixture is washed with aqueous sodiumcarbonate twice, 40% aqu. sodium bisulfite and water. The organic phase is dried (MgSO4) and evaporated. The residue is recrystallised from ethanol (12 g) to obtain N-(2′,6′-Dichlorophenyl)-N-chloroacetyl (2.83 g), mp: 129.5-130° C.

후처리

  1. washAfter dilution with toluene, the mixture is washed with aqueous sodiumcarbonate twice
  2. dry with materialThe organic phase is dried (MgSO4)
  3. customevaporated
  4. customThe residue is recrystallised from ethanol (12 g)
  5. customto obtain N-(2′,6′-Dichlorophenyl)-N-chloroacetyl (2.83 g), mp: 129.5-130° C.

출처 및 근거

ORD 기록
ord-956fed54a7fb4ecaa4fe37157e1534b6
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07906677B2

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