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

HRID 727854ノート

反応式

HRID 727854 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-84c8a2d813d8415892ee96a287f42d37
出典データセット
uspto-grants-1991_09
特許番号
US05045558

反応ノート

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