تفاعل #66609

ord-e4d2cf8e077f4252a86e82a5fa114462

ظروف التفاعل

درجة الحرارة
50°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe vessel was capped
  2. 2
    درجة الحرارةAfter 16 hours the solution was cooled to room temperature
  3. 3
    أخرىevaporated
  4. 4
    استخلاصThe mixture was extracted with ethyl acetate
  5. 5
    غسيلwashed with H2O
  6. 6
    غسيلwashed with brine
  7. 7
    تجفيفThe combined organic layers were dried over Na2SO4
  8. 8
    ترشيحfiltered
  9. 9
    أخرىevaporated in vacuo
  10. 10
    أخرىPurification via flash chromatography (4:1 hexane/ethyl acetate)

الإجراء التجريبي

To a glass pressure vessel containing 4-chloro-5-(2-isopropyl-4,5-dimethoxy-benzyl)-2-methylsulfanyl-pyrimidine (0.212 g, 0.6 mmol) was added 5.0 mL ethyl amine via a cold finger condenser. The vessel was capped and warmed to 50° C. After 16 hours the solution was cooled to room temperature, evaporated and taken up in H2O. The mixture was extracted with ethyl acetate, washed with H2O and then washed with brine. The combined organic layers were dried over Na2SO4, filtered and evaporated in vacuo. Purification via flash chromatography (4:1 hexane/ethyl acetate) afforded ethyl-[5-(2-isopropyl-4,5-dimethoxy-benzyl)-2-methylsulfanyl-pyrimidin-4-yl]-amine (0.136 g, 63%) as a white solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08524725B2uspto-grants-2013_09