Water → HCID 23508546, 화합물

HRID 1883674노트

반응식

HRID 1883674 반응식
[CH3:1][O:2][C:3]1[CH:19]=[CH:18][C:6]([C:7]([NH:9][C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=2)=[O:8])=[CH:5][CH:4]=1.[H-].[Na+].[CH2:22](I)[CH3:23].O>CS(C)=O>[CH2:22]([N:9]([C:10]1[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=1)[C:7](=[O:8])[C:6]1[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:19][CH:18]=1)[CH3:23]

참가 물질

6

반응물 4

HCID 962WaterHCID 6340IodoethaneHCID 24758Sodium hydrideHCID 3468154-Methoxy-N-(4-methoxyphenyl)benzamide

생성물 1

HCID 23508546HCID 23508546, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

A mixture composed of 600 mg of 4-methoxy-N-(4-methoxy-phenyl)benzamide and 150 mg of 60% sodium hydride was stirred in 7.5 ml of dimethyl sulfoxide at 50° C. for 10 minutes. Then, 1.05 ml of ethyl iodide was added, and the reaction mixture was stirred for 30 minutes. After water was added to the reaction mixture, the product was extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous sodium sulfate. After the solvent was distilled off, the resulting crude product was purified by TLC (using a 80:1 mixture of chloroform and acetone as the developing solvent) to obtain 591 mg of N-ethyl-4-methoxy-N-(4-methoxyphenyl)benzamide.

후처리

  1. extractionthe product was extracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationAfter the solvent was distilled off
  5. customthe resulting crude product was purified by TLC (
  6. additiona 80:1 mixture of chloroform and acetone as the developing solvent)

출처 및 근거

ORD 기록
ord-492c8d4c3da241919cfaef9dbab8a747
출처 데이터셋
uspto-grants-2004_07
특허 번호
US06762205B1

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