Methylamine → N,3,4-Trimethylbenzamide

HRID 1078347ノート

反応式

HRID 1078347 の反応式
[CH3:1][NH2:2].[CH3:3][C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=1[CH3:13])[C:7](Cl)=[O:8]>O1CCCC1>[CH3:1][NH:2][C:7](=[O:8])[C:6]1[CH:10]=[CH:11][C:12]([CH3:13])=[C:4]([CH3:3])[CH:5]=1

参加物

4

反応物 2

HCID 6329MethylamineHCID 27585353,4-Dimethylbenzoyl chloride

生成物 1

HCID 3341433N,3,4-Trimethylbenzamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

108 ml of a 40% strength aqueous solution of methylamine were dissolved in 300 ml of tetrahydrofuran. 53 g of 3,4-dimethylbenzoyl chloride were added dropwise to this solution with ice cooling. The reaction mixture was subsequently stirred at room temperature for 1 hour. Then the reaction mixture was concentrated to half its volume under reduced pressure, saturated sodium chloride solution was added, and the mixture was acidified with concentrated hydrochloric acid. The product which then precipitated was filtered out with suction and dried at 40° C. over potassium hydroxide in a drying cabinet. 47 g of N-methyl-3,4-dimethylbenzamide were obtained.

後処理

  1. concentrationThen the reaction mixture was concentrated to half its volume under reduced pressure, saturated sodium chloride solution
  2. additionwas added
  3. customThe product which then precipitated
  4. filtrationwas filtered out with suction
  5. dry with materialdried at 40° C. over potassium hydroxide in a drying cabinet

出典と根拠

ORDレコード
ord-8b73b12c5bbf4a9789095c3c8301a1ee
出典データセット
uspto-grants-1996_08
特許番号
US05547967

反応ノート

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