تفاعل #303544

ord-eef7da6afb894142967b5ee27be5ba2e

المذيبات

ظروف التفاعل

درجة الحرارة
70°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىvolatiles were removed
  2. 2
    أخرىThe residue was partitioned between diethyl ether and 1 N hydrochloric acid
  3. 3
    غسيلThe aqueous phase was washed with diethyl ether
  4. 4
    استخلاصextracted with ethyl acetate
  5. 5
    غسيلThe combined organic extracts were washed with brine
  6. 6
    تجفيفdried (sodium sulfate)
  7. 7
    تركيزconcentrated in vacuo

الإجراء التجريبي

Hydrogen chloride (4 M in 1,4-dioxane) (5.25 mL, 21 mmol) was added to an ambient temperature solution of 1-[4-(2,2-dimethylpropyl)-1-trityl-1H-imidazol-2-yl]-2-[4-(1-methyl-1H-pyrazol-4-yl)phenyl]propan-2-ol (250 mg, 0.42 mmol) in methanol (10 mL). After stirring at 70° C. for 1 h, volatiles were removed. The residue was partitioned between diethyl ether and 1 N hydrochloric acid. The aqueous phase was washed with diethyl ether, basified with 2.5 N aqueous sodium hydroxide and extracted with ethyl acetate. The combined organic extracts were washed with brine, dried (sodium sulfate) and concentrated in vacuo to afford the title compound. (M+H) found 339.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08193228B2uspto-grants-2012_06