Chloroacetyl chloride → N-(2'-Chloro-6'-methylphenyl)-N-chloroacetyl-4-methylaniline

HRID 603343

반응식

HRID 603343 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[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]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[N:9]([C:19](=[O:20])[CH2:18][Cl:17])[C:10]1[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][CH:11]=1

참가 물질

4

반응물 2

HCID 6577Chloroacetyl chlorideHCID 57952145N-(2'-chloro-6'-methylphenyl)-4-methylaniline

생성물 1

HCID 57952152N-(2'-Chloro-6'-methylphenyl)-N-chloroacetyl-4-methylaniline수율 77.9%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

The solution of N-(2′-chloro-6′-methylphenyl)-4-methylaniline (1.4 g) in 2.21 g chloroacetylchloride is heated to 90° C. for 4 h. The mixture is diluted with toluene (25 ml), cooled to room temperature and washed with aqu. sodium carbonate. The organic phase is dried, evaporated and the residue is subjected to flash chromatography [57 g silica, toluene and toluene/ethylacetate (98:2)] to afford 1.45 g of N-(2′-Chloro-6′-methylphenyl)-N-chloroacetyl-4-methylaniline which is crystallised from heptane, mp: 113-114° C.

후처리

  1. washwashed with aqu
  2. customThe organic phase is dried
  3. customevaporated

출처 및 근거

ORD 기록
ord-a3456b5d6a45462da116fb640b9a79d2
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07906677B2

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