Pyridine → N-(4-bromo-2-chlorophenyl)-3-chloropropanamide

HRID 1774841ノート

反応式

HRID 1774841 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[C:4]([Cl:9])[CH:3]=1.N1C=CC=CC=1.[Cl:16][CH2:17][CH2:18][C:19](Cl)=[O:20]>C(Cl)Cl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:19](=[O:20])[CH2:18][CH2:17][Cl:16])=[C:4]([Cl:9])[CH:3]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 693643-Chloropropionyl chlorideHCID 6101694-Bromo-2-chloroaniline

生成物 1

HCID 43346898N-(4-bromo-2-chlorophenyl)-3-chloropropanamide収率 90%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4-bromo-2-chloro-phenylamine (32 g, 0.15 mol) and pyridine (13.45 g, 0.17 mol) in DCM (200 mL) was added 3-chloropropionyl chloride (21.65 g, 0.17 mol) dropwise at 15° C. After stirring at room temperature for 1 hour, the mixture was washed with water and then hydrochloric acid (2 N, aqueous). The organic layer was dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to afford title compound (10.9 g, yield: 90%) as a white solid.

後処理

  1. washthe mixture was washed with water
  2. dry with materialThe organic layer was dried over anhydrous Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-376d4e64907a4af691c7f643a8dc1947
出典データセット
uspto-grants-2016_02
特許番号
US09260408B2

反応ノート

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