تفاعل #516985

ord-885f933a31d248f6b6e4ab3e4df96001

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىevaporated in vacuo to dryness
  2. 2
    workup.ADDITIONThe residue is treated with 60 ml of water and 5N HCl
  3. 3
    أخرىto obtain a pH of 2
  4. 4
    أخرىthe solid collected
  5. 5
    غسيلwashed
  6. 6
    أخرىdried
  7. 7
    درجة الحرارةin refluxing acetone
  8. 8
    أخرىcollected again

الإجراء التجريبي

5.33 g (20 mmoles) of 8-cyclopropyl-3-n-propyl-2,6-dithioxantine and 42 ml of cyclopentylamine were heated in a 450 ml pressure reactor to 150° C. (50 psi) with the exclusion of air. After 20 hours the solution was transferred with menthol to a round bottom flask and evaporated in vacuo to dryness. The residue is treated with 60 ml of water and 5N HCl to obtain a pH of 2. The suspension is neutralized with bicarbonate to pH 7, the solid collected, washed, dried, suspended in refluxing acetone and collected again: 5.98 g of thioisoguanine with mp 274-6° C. (decomp).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06319928B1uspto-grants-2001_11