N,N-dimethyl-p-phenylenediamine → HCID 68154733, 화합물

HRID 1020015노트

반응식

HRID 1020015 반응식
CO[CH:3]=[C:4]([C:11]([O:13][CH3:14])=[O:12])[CH:5]=[CH:6][C:7]([O:9]C)=O.[CH3:15][N:16]([CH3:24])[C:17]1[CH:23]=[CH:22][C:20]([NH2:21])=[CH:19][CH:18]=1>CN(C=O)C>[CH3:15][N:16]([CH3:24])[C:17]1[CH:23]=[CH:22][C:20]([N:21]2[C:7](=[O:9])[CH:6]=[CH:5][C:4]([C:11]([O:13][CH3:14])=[O:12])=[CH:3]2)=[CH:19][CH:18]=1

참가 물질

4

반응물 2

HCID 7472N,N-dimethyl-p-phenylenediamineHCID 71338068Dimethyl 4-(methoxymethylidene)pent-2-enedioate

생성물 1

HCID 68154733HCID 68154733, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
50 °C

실험 절차

After 1.24 g (6.1 mmol) of dimethyl 4-(methoxymethylene)2-pentenedioate obtained in Example 1-1 was dissolved in 10 mL of DMF, 830 g (6.1 mmol) of 4-dimethylaminoaniline was added to the solution. Afterward, the resulting reaction solution was stirred under reflex at about 50° C. for about 3 hours. After termination of the reaction was determined by liquid chromatography, the solvent was removed in vacuo and was then washed using brine, followed by drying using magnesium sulfate and filtration. After distillation under reduced pressure, the resulting product was purified using column chromatography (hexane:ethyl acetate=1:1) to obtain a target compound (Actual yield: 357 mg, Yield ratio: 21%).

후처리

  1. customAfterward, the resulting reaction solution
  2. customthe solvent was removed in vacuo
  3. washwas then washed
  4. customby drying
  5. filtrationmagnesium sulfate and filtration
  6. distillationAfter distillation under reduced pressure
  7. customthe resulting product was purified
  8. customto obtain
  9. customa target compound (Actual yield: 357 mg, Yield ratio: 21%)

출처 및 근거

ORD 기록
ord-e702e65d08a74266a6baf9ced7c06115
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716309B2

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