Hydrochloric Acid → 4-[1-(1-Imidazolyl)-butyl]-benzoic acid cyclohexyl ester

HRID 727854노트

반응식

HRID 727854 반응식
[N:1]1([CH:6]([C:10]2[CH:18]=[CH:17][C:13]([C:14]([OH:16])=[O:15])=[CH:12][CH:11]=2)[CH2:7][CH2:8][CH3:9])[CH:5]=[CH:4][N:3]=[CH:2]1.[CH:19]1(O)[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1.N1C=CC=CC=1.Cl>C(Cl)Cl>[CH:19]1([O:15][C:14](=[O:16])[C:13]2[CH:17]=[CH:18][C:10]([CH:6]([N:1]3[CH:5]=[CH:4][N:3]=[CH:2]3)[CH2:7][CH2:8][CH3:9])=[CH:11][CH:12]=2)[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 7966CyclohexanolHCID 145143684-[1-(1-Imidazolyl)-butyl]-benzoic acid

생성물 1

HCID 541855554-[1-(1-Imidazolyl)-butyl]-benzoic acid cyclohexyl ester수율 78%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1 g of 4-[1-(1-imidazolyl)-butyl]-benzoic acid is converted, analogously to example 20, into the acid chloride; it is dissolved in 10 ml of methylene chloride, mixed with 360 mg of cyclohexanol and 3 ml of pyridine, after 20 hours at room temperature it is added to excess 1M hydrochloric acid and extracted with ether. The water phase is alkalized with potassium carbonate and extracted with ethyl acetate. After drying and concentration by evaporation, the residue is distilled on a bulb tube. 915 mg of the title compound is obtained as oil with a boiling point of 200° C./0.03 mbar.

후처리

  1. extractionextracted with ether
  2. extractionextracted with ethyl acetate
  3. customAfter drying
  4. concentrationconcentration
  5. customby evaporation
  6. distillationthe residue is distilled on a bulb tube

출처 및 근거

ORD 기록
ord-84c8a2d813d8415892ee96a287f42d37
출처 데이터셋
uspto-grants-1991_09
특허 번호
US05045558

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