Water → 4'-Dimethylaminoacetanilide

HRID 2093040

반응식

HRID 2093040 반응식
[CH3:1][N:2]([CH3:10])[C:3]1[CH:8]=[CH:7][C:6]([NH2:9])=[CH:5][CH:4]=1.C(N(CC)CC)C.[C:18](OC(=O)C)(=[O:20])[CH3:19].O>ClCCl>[CH3:1][N:2]([CH3:10])[C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:18](=[O:20])[CH3:19])=[CH:5][CH:4]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 7472N,N-dimethyl-p-phenylenediamineHCID 7918Acetic AnhydrideHCID 8471Triethylamine

생성물 1

HCID 819684'-Dimethylaminoacetanilide수율 69%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of N,N-dimethylbenzene-1,4-diamine (1.0 eq) in dichloromethane, triethylamine (2.2 eq) was added at 0° C. and stirred for 15 min. To the above mixture was then added a solution of acetic anhydride (1.0 eq) in dichloromethane at 0° C., after addition the reaction was continued at room temperature for 5 hrs. Water was added and the organic layer was separated, dried over anhydrous Na2SO4, concentrated under reduced pressure to afford crude product, which, on purification by column chromatography afforded the desired N-[4-(dimethylamino)phenyl]acetamide. (Yield=69%)

후처리

  1. additionafter addition the reaction
  2. waitwas continued at room temperature for 5 hrs
  3. customthe organic layer was separated
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated under reduced pressure
  6. customto afford crude product, which
  7. customon purification by column chromatography

출처 및 근거

ORD 기록
ord-caed95fe1a9247fd8670bf899b7624dc
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08440830B2

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