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

HRID 555257

반응식

HRID 555257 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9b239ee410874131801acfbc5a613f8b
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08053441B2

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