Methylamine → N,3,4-Trimethylbenzamide

HRID 1078347노트

반응식

HRID 1078347 반응식
[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

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 27585353,4-Dimethylbenzoyl chloride

생성물 1

HCID 3341433N,3,4-Trimethylbenzamide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8b73b12c5bbf4a9789095c3c8301a1ee
출처 데이터셋
uspto-grants-1996_08
특허 번호
US05547967

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