تفاعل #77215

ord-ede405ec21084346b6e3a0daa2d97f5b

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe resulting reaction mixture
  2. 2
    درجة الحرارةwas refluxed
  3. 3
    استخلاصextracted with EtOAc until the aqueous layer
  4. 4
    تجفيفThe combined organics were dried over MgSO4
  5. 5
    تركيزconcentrated on rotary evaporator
  6. 6
    أخرىThe desired product was purified by silica gel flash chromatography

الإجراء التجريبي

To a solution of 4-Piperazin-1-ylmethyl-benzoic acid (4c) and chloro-(dimethyl-phosphinoyl)-methane (5a) in ethanol was added potassium carbonate. The resulting reaction mixture was refluxed, then cooled to room temperature, diluted with brine, acidified to pH-4, and extracted with EtOAc until the aqueous layer showed little or no evidence of product by HPLC. The combined organics were dried over MgSO4 and concentrated on rotary evaporator. The desired product was purified by silica gel flash chromatography.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06706699B2uspto-grants-2004_03