تفاعل #215126

ord-1d85b24c53974f18bd577b30b6e9f217

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAfter 1 hour of reaction at room temperature
  2. 2
    أخرىA reddish syrup, 2.2 g which is formed in the bottom of the flask
  3. 3
    أخرىis isolated by decantation
  4. 4
    أخرىThe product may be purified
  5. 5
    أخرىThe reddish syrup obtained
  6. 6
    استخلاصto extract the product
  7. 7
    تجفيفAfter dried over anhydrous sodium sulfate the chloroform solution which
  8. 8
    أخرىis evaporated at 35° C. in vacuum

الإجراء التجريبي

6-Aminonicotinamide 1.37 g (0.01 mole) is dissolved in 10 ml of 2-pyrrolidinone and 3 ml of pyridine by gentle warming of the mixture. Diphenylphosphoryl chloride 6 ml (0.024 mole) is then slowly added to the mixture. After 1 hour of reaction at room temperature, the mixture is poured into 300 ml of 0.2 N HCl. A reddish syrup, 2.2 g which is formed in the bottom of the flask is isolated by decantation. The product may be purified as follows. The reddish syrup obtained above is dissolved in 3 ml of ethanol and the solution is admixed with 200 ml of 0.2 N HCl. Chloroform, 100 ml is added to the mixture to extract the product. After dried over anhydrous sodium sulfate the chloroform solution which contains the product is evaporated at 35° C. in vacuum to give a practically pure 6-diphenylphosphorylamino nicotinamide.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04258052uspto-grants-1981_03