Acetic Anhydride → N-(3-Bromo-4-methylphenyl)acetamide

HRID 29819

反応式

HRID 29819 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][C:8]=1[CH3:9])[NH2:5].[C:10](OC(=O)C)(=[O:12])[CH3:11]>C(Cl)Cl>[C:10]([NH:5][C:4]1[CH:6]=[CH:7][C:8]([CH3:9])=[C:2]([Br:1])[CH:3]=1)(=[O:12])[CH3:11]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 82187Benzenamine, 3-bromo-4-methyl-

生成物 1

HCID 11708413N-(3-Bromo-4-methylphenyl)acetamide収率 99.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 3-bromo-4-methylaniline (1.27 g, 6.82 mmol) in DCM (20 mL) at (0° C. is added acetic anhydride (0.676 mL, 7.16 mmol) dropwise. After 30 minutes, the mixture is partitioned between DCM and saturated sodium carbonate solution. The layer is separated and the aqueous layer is extracted with DCM. The combined organic extracts are washed with brine, dried over Na2SO4, filtered and concentrated to afford the title compound (1.55 g, 99%). The residue is used in the next step without further purification.

後処理

  1. customthe mixture is partitioned between DCM and saturated sodium carbonate solution
  2. customThe layer is separated
  3. extractionthe aqueous layer is extracted with DCM
  4. washThe combined organic extracts are washed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-b205cd67cc5f4963b841b1479888a34a
出典データセット
uspto-grants-2008_09
特許番号
US07423038B2

関連ノート

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