تفاعل #44525

ord-ee4c67b25ee64efdb3c0893c80b0defa

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooled
  2. 2
    تركيزconcentrated
  3. 3
    workup.ADDITIONtreated with water
  4. 4
    استخلاصextracted with ethyl acetate
  5. 5
    غسيلThe extract was washed with brine
  6. 6
    تجفيفdried over anhydrous sodium sulfate
  7. 7
    تركيزconcentrated
  8. 8
    أخرىThe concentrate was triturated with ethyl ether
  9. 9
    ترشيحfiltered

الإجراء التجريبي

A mixture of 4-chloro-2-methylsulfanylpyrimidine (8 g) and 7N ammonia in methanol (100 mL) at 100° C. was stirred for 2 days in a sealed tube, cooled, concentrated, treated with water, and extracted with ethyl acetate. The extract was washed with brine, dried over anhydrous sodium sulfate, and concentrated. The concentrate was triturated with ethyl ether and filtered. 1H NMR (300 MHz, CDCl3) δ 8.06 (d, 1H), 6.12 (d, 1H), 4.83 (s, 2H), 2.51 (s, 3H).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07737159B2uspto-grants-2010_06