N-(4-dimethylaminomethylphenylmethyl)acetamide → 4-Dimethylaminomethylbenzylamine

HRID 1595378노트

반응식

HRID 1595378 반응식
[CH3:1][N:2]([CH2:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][NH:12]C(=O)C)=[CH:7][CH:6]=1)[CH3:3]>Cl>[CH3:3][N:2]([CH2:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][NH2:12])=[CH:7][CH:6]=1)[CH3:1]

참가 물질

3

반응물 1

HCID 21703715N-(4-dimethylaminomethylphenylmethyl)acetamide

생성물 1

HCID 1937144-Dimethylaminomethylbenzylamine수율 66.8%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

N-(4-Dimethylaminomethylphenylmethyl)acetamide (22 g) was dissolved in 4N hydrochloric acid (100 ml) and the mixture was refluxed under heating for 3 hr 40 min. The solvent was evaporated and ethyl acetate was added. The resulting crystals were collected by filtration. The obtained crystals were dissolved in water (40 ml) and potassium carbonate was added to saturation, and the mixture was extracted with chloroform. The extract was dried over anhydrous sodium sulfate and, after drying, the solvent was evaporated under reduced pressure to give the objective 4-(dimethylaminomethyl)phenylmethylamine (11.7 g), melting point 38-39° C.

후처리

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 3 hr 40 min
  3. customThe solvent was evaporated
  4. additionethyl acetate was added
  5. filtrationThe resulting crystals were collected by filtration
  6. dissolutionThe obtained crystals were dissolved in water (40 ml)
  7. additionpotassium carbonate was added to saturation
  8. extractionthe mixture was extracted with chloroform
  9. dry with materialThe extract was dried over anhydrous sodium sulfate
  10. customafter drying
  11. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-7a3488afb51e4d84b089cd3ba7d292f4
출처 데이터셋
uspto-grants-2001_09
특허 번호
US06288061B1

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