تفاعل #2207370

ord-42ca336bca1c4b0db50b5b1739f07814

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
55°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITput aside at room temperature for 3 hours
  2. 2
    درجة الحرارةthe mixture is cooled to 5° C.
  3. 3
    أخرىthe separated solid is collected
  4. 4
    workup.DISSOLUTIONdissolved in 10% sodium carbonate solution
  5. 5
    ترشيحAny insoluble material is filtered off
  6. 6
    أخرىThe solid is collected
  7. 7
    غسيلwashed with water
  8. 8
    أخرىdried

الإجراء التجريبي

To a solution of 8.27 g (0.04 mol) of the compound obtained in Example 4 in 39.4 ml of glacial acetic acid there are added, with sting, 25 ml of water, and to this solution there is slowly added a solution of 6.54 g of potassium cyanate in 10 ml of water. Once a white precipitate appears, the remaining potassium cyanate solution is added in one portion immediately. The mixture is warmed at 55° C., and stirred for 1 hour, then put aside at room temperature for 3 hours. 50 ml of water are added and the mixture is cooled to 5° C.; the separated solid is collected and dissolved in 10% sodium carbonate solution. Any insoluble material is filtered off and the filtrate is acidified with dilute sulphuric acid. The solid is collected and washed with water and dried, giving the title compound.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06689808B2uspto-grants-2004_02