تفاعل #66609
ord-e4d2cf8e077f4252a86e82a5fa114462
معادلة التفاعل
الكواشف
لا شيء
ظروف التفاعل
درجة الحرارة
50°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىThe vessel was capped
- 2درجة الحرارةAfter 16 hours the solution was cooled to room temperature
- 3أخرىevaporated
- 4استخلاصThe mixture was extracted with ethyl acetate
- 5غسيلwashed with H2O
- 6غسيلwashed with brine
- 7تجفيفThe combined organic layers were dried over Na2SO4
- 8ترشيحfiltered
- 9أخرىevaporated in vacuo
- 10أخرىPurification 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.