Triethylamine → 3-(4-Tert-butylphenyl)-5,5-dimethyl-imidazolidine-2,4-dione

HRID 546554

반응식

HRID 546554 반응식
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([N:11]=[C:12]=[O:13])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.Cl.C[O:23][C:24](=O)[C:25]([CH3:28])([CH3:27])[NH2:26]>C1(C)C=CC=CC=1>[C:1]([C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C:24](=[O:23])[C:25]([CH3:28])([CH3:27])[NH:26][C:12]2=[O:13])=[CH:7][CH:6]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 27356951-Tert-butyl-4-isocyanatobenzeneHCID 13258034Methyl 2-aminoisobutyrate hydrochloride

생성물 1

HCID 576259723-(4-Tert-butylphenyl)-5,5-dimethyl-imidazolidine-2,4-dione수율 79.6%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a suspension of 15 g of 4-tert-butylphenyl-isocyanate in 200 mL of toluene are successively added 31.52 mL of triethylamine and 13.15 g of 2,2-dimethylglycine methyl ester hydrochloride. The reaction mixture is refluxed for 24 h, cooled to room temperature, poured into distilled water and extracted with ethyl acetate. The organic phase is washed successively with water and with saturated sodium chloride solution, dried over magnesium sulphate, filtered and concentrated under reduced pressure. The residue is taken up in diethyl ether and the solid formed is filtered off and dried to give 17.75 g of 3-(4-tert-butylphenyl)-5,5-dimethyl-imidazolidine-2,4-dione, the characteristics of which are as follows:

후처리

  1. temperatureThe reaction mixture is refluxed for 24 h
  2. additionpoured
  3. distillationinto distilled water
  4. extractionextracted with ethyl acetate
  5. washThe organic phase is washed successively with water and with saturated sodium chloride solution
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customthe solid formed
  10. filtrationis filtered off
  11. customdried

출처 및 근거

ORD 기록
ord-d90c02ee6adf431e9a8831060f8eba9f
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07935819B2

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