15-Crown-5 → HCID 178447070, 화합물

HRID 1067663노트

반응식

HRID 1067663 반응식
C1(C(C2C=CC=CC=2)(C2C=CC=CC=2)[N:8]2[CH:12]=[C:11]([CH2:13][CH2:14][CH2:15][O-:16])[N:10]=[CH:9]2)C=CC=CC=1.[Na+].[Br-].[CH3:31][CH:32]([CH3:35])[CH2:33][CH3:34].O1CCOCCOCCOCCOCC1>C1(C)C=CC=CC=1>[CH3:31][CH:32]([CH3:35])[CH2:33][CH2:34][O:16][CH2:15][CH2:14][CH2:13][C:11]1[N:10]=[CH:9][NH:8][CH:12]=1

참가 물질

5

반응물 3

HCID 3633615-Crown-5HCID 211936043-Methylbutane bromideHCID 23682245sodium 3-(1-triphenylmethyl-1H-imidazol-4-yl)propanolate

생성물 1

HCID 178447070HCID 178447070, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
70 °C

실험 절차

5 mmol of sodium 3-(1-triphenylmethyl-1H-imidazol-4-yl)propanolate, 5 mmol of 3-methylbutane bromide and 0.5 mmol of 15-crown-15 (1, 4, 7, 10, 13-pentaoxacyclopentadecane) dissolved in 10 ml of anhydrous toluene are refluxed for 24 hours. The solvent is then evaporated off, and the residue dissolved in 10 ml THF and 30 ml 2N HCl and then heated at 70° C. for 2 hours. The THF is evaporated off under reduced pressure and triphenylmethanol is extracted with diethyl ether. The aqueous phase is neutralized with potassium carbonate and the product is extracted with diethyl ether. The organic extract is dried and evaporated, giving rise to an oil, which is crystallized as hydrogen maleate from diethyl ether and ethanol.

후처리

  1. temperatureare refluxed for 24 hours
  2. customThe solvent is then evaporated off
  3. dissolutionthe residue dissolved in 10 ml THF
  4. customThe THF is evaporated off under reduced pressure and triphenylmethanol
  5. extractionis extracted with diethyl ether
  6. extractionthe product is extracted with diethyl ether
  7. extractionThe organic extract
  8. customis dried
  9. customevaporated
  10. customgiving rise to an oil, which
  11. customis crystallized as hydrogen maleate from diethyl ether and ethanol

출처 및 근거

ORD 기록
ord-591bdee9a8134fd883b97e6fd5bd97c6
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06248765B1

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