Hydrochloric Acid → HCID 178446745, 화합물

HRID 1067699

반응식

HRID 1067699 반응식
[CH3:1][C:2]([CH3:8])([CH2:6][CH3:7])C(O)=O.C([N:11]([CH2:14]C)CC)C.P(N=[N+]=[N-])(=O)(OC1C=CC=CC=1)[O:17]C1C=CC=CC=1.[NH:35]1[CH:39]=[C:38]([CH2:40][CH2:41][CH2:42][OH:43])[N:37]=[CH:36]1.Cl>C(#N)C>[CH3:8][C:2]([NH:11][C:14](=[O:17])[O:43][CH2:42][CH2:41][CH2:40][C:38]1[N:37]=[CH:36][NH:35][CH:39]=1)([CH2:6][CH3:7])[CH3:1]

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 116842,2-Dimethylbutanoic acidHCID 123414Diphenylphosphoryl azideHCID 178520509HCID 178520509, 화합물

생성물 1

HCID 178446745HCID 178446745, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

5 mmol of 2,2-dimethylbutyric acid, 5 mmol of triethylamine and 5 mmol of diphenyl phosphorazidate in 30 ml of anhydrous acetonitrile are stirred at 20° C. for 45 minutes and are then brought to reflux for 30 minutes. 6 mmol of 3-(1H-imidazol-4-yl)propanol.HCl are added and are brought to reflux for 40 hours. The mixture is evaporated and the residue dissolved in diethyl ether. The solution is washed successively with 30 ml of 5% aqueous citric acid, 30 ml of H2O and 30 ml of saturated aqueous NaHCO3. The organic layer is evaporated and the residue is purified by rotatory chromatography (eluent: chloroform/methanol (99:1-90:10)). After removal of the solvent under reduced pressure, the residue is crystallized in the form of hydrogen oxalate in diethyl ether and ethanol.

후처리

  1. temperatureto reflux for 30 minutes
  2. temperatureto reflux for 40 hours
  3. customThe mixture is evaporated
  4. dissolutionthe residue dissolved in diethyl ether
  5. washThe solution is washed successively with 30 ml of 5% aqueous citric acid, 30 ml of H2O and 30 ml of saturated aqueous NaHCO3
  6. customThe organic layer is evaporated
  7. customthe residue is purified by rotatory chromatography (eluent: chloroform/methanol (99:1-90:10))
  8. customAfter removal of the solvent under reduced pressure
  9. customthe residue is crystallized in the form of hydrogen oxalate in diethyl ether and ethanol

출처 및 근거

ORD 기록
ord-b94b80b7c4884ad0baea7653797b1fe0
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06248765B1

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