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

HRID 603348

反応式

HRID 603348 の反応式
[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

参加物

3

反応物 2

HCID 6577Chloroacetyl chlorideHCID 57952151N-(2',6'-Dichlorophenyl)-4-methylaniline

生成物 1

HCID 57952147N-(2',6'-dichlorophenyl)-N-chloroacetyl-4-methylaniline

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-956fed54a7fb4ecaa4fe37157e1534b6
出典データセット
uspto-grants-2011_03
特許番号
US07906677B2

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