Dichloromethane → 5-Chloro-2-(2-methyl-acryloylamino)-benzamide

HRID 555257

反応式

HRID 555257 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:3]=1[C:4]([NH2:6])=[O:5].C[CH:13]=[CH:14][C:15](Cl)=[O:16].[CH2:18](Cl)Cl>>[Cl:11][C:8]1[CH:9]=[CH:10][C:2]([NH:1][C:15](=[O:16])[C:14]([CH3:18])=[CH2:13])=[C:3]([CH:7]=1)[C:4]([NH2:6])=[O:5]

参加物

4

反応物 3

HCID 6344DichloromethaneHCID 788762-Amino-5-chlorobenzamideHCID 790802-Butenoyl chloride

生成物 1

HCID 589496945-Chloro-2-(2-methyl-acryloylamino)-benzamide

実験手順

2-Amino-5-chloro-benzamide (2.5 mmoL), a literature known compound, was treated with TEA (3.0 mmoL) followed by methylacryl chloride (2.5 mmoL) in DCM at 0° C. The reaction was slowly warmed to room temperature and kept for another 2 h. The reaction mixture was then partitioned between DCM and water. The organic layer was washed with sat. Na2CO3, brine, dried over anhydrous Na2SO4, filtered, concentrated and purified by silica gel column chromatography to afford the title compound as a white solid.

後処理

  1. additionwas treated with TEA (3.0 mmoL)
  2. customThe reaction mixture was then partitioned between DCM and water
  3. washThe organic layer was washed with sat. Na2CO3, brine
  4. dry with materialdried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. custompurified by silica gel column chromatography

出典と根拠

ORDレコード
ord-9b239ee410874131801acfbc5a613f8b
出典データセット
uspto-grants-2011_11
特許番号
US08053441B2

関連ノート

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