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

HRID 603343

反応式

HRID 603343 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-a3456b5d6a45462da116fb640b9a79d2
出典データセット
uspto-grants-2011_03
特許番号
US07906677B2

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