Pyridine → N-Methoxy-N,4-dimethylbenzamide

HRID 1271262

반응식

HRID 1271262 반응식
[C:1]1([CH3:10])[CH:6]=[CH:5][C:4]([C:7](Cl)=[O:8])=[CH:3][CH:2]=1.Cl.[CH3:12][NH:13][O:14][CH3:15].N1C=CC=CC=1>ClCCl>[CH3:15][O:14][N:13]([CH3:12])[C:7]([C:4]1[CH:5]=[CH:6][C:1]([CH3:10])=[CH:2][CH:3]=1)=[O:8]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 134054-Methylbenzoyl ChlorideHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)

생성물 1

HCID 5133773N-Methoxy-N,4-dimethylbenzamide수율 89.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 10.00 g of p-toluoyl chloride in 300 ml of dichloromethane, 6.94 g of N,O-dimethylhydroxyamine hydrochloride was added. The reaction solution was ice-cooled and 11.5 ml of pyridine was added dropwise. After the completion of dropwise addition, the mixture was stirred at room temperature for one hour and the solvent was evaporated under reduced pressure. The residue was combined with water, extracted with diethyl ether and then washed in turn with 10% hydrochloric acid, water and an aqueous saturated sodium hydrogen carbonate solution. After drying over anhydrous magnesium sulfate, the solvent was evaporated under reduced pressure to obtain 10.40 g of the desired compound as a colorless oily substance.

후처리

  1. temperaturecooled
  2. additionAfter the completion of dropwise addition
  3. customthe solvent was evaporated under reduced pressure
  4. extractionextracted with diethyl ether
  5. washwashed in turn with 10% hydrochloric acid, water
  6. dry with materialAfter drying over anhydrous magnesium sulfate
  7. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-04e4233c137646ee8cd244384cd648f1
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07205302B2

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