تفاعل #54486

ord-2ea726274d5b438283d3b7d1fe3bc327

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas maintained at the boil for 40 hours
  2. 2
    درجة الحرارةAfter cooling
  3. 3
    غسيلwashed three times with water
  4. 4
    أخرىThe resinous residue of the organic phase was chromatographed
  5. 5
    غسيلThe base was eluted as a resin
  6. 6
    أخرىtheoretical yield)

الإجراء التجريبي

A stirred mixture of 8 g (0.02 mol) of 1-phenyl-2-(1-piperazinyl)-indole 3-carboxylic acid (4-methyl)-piperazide, 9.45 g (0.07 mol) of 2-(2-chloroethyl)-1,3-dioxolane and 9.7 ml of triethylamine in 60 ml of toluene was maintained at the boil for 40 hours. After cooling, the mixture was diluted with 200 ml of chloroform, washed three times with water, and the solvent was eliminated in vacuo. The resinous residue of the organic phase was chromatographed using silica gel 60 (0.06-0.2 mm, deactivated by 10% of water, column size: 3 × 100 cm) with chloroform containing 10% methanol. The base was eluted as a resin. The yield amounted to 6.6 g (66% of the theoretical yield). The dihydrochloride melted at 215°-217° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04148895uspto-grants-1979_04