تفاعل #66653

ord-66d5cef76407439694107f0cd2e116ff

المذيبات

ظروف التفاعل

درجة الحرارة
85°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter 3 days the solution was cooled
  2. 2
    تركيزconcentrated in vacuo
  3. 3
    ترشيحThe precipitate was filtered
  4. 4
    تركيزthe mother liquor was concentrated in vacuo
  5. 5
    أخرىPurification via flash chromatography (7:3 hexane/ethyl acetate)

الإجراء التجريبي

To 25 ml of saturated NH3 in EtOH was added 4-Chloro-5-(5-chloro-2-isopropyl-4-methoxy-benzyl)-2-methylsulfanyl-pyrimidine (0.580 g, 1.6 mmol). The solution was warmed to 85° C. in a sealed reaction vessel. After 3 days the solution was cooled, concentrated in vacuo and suspended in CH2Cl2. The precipitate was filtered and the mother liquor was concentrated in vacuo. Purification via flash chromatography (7:3 hexane/ethyl acetate) afforded 5-(5-chloro-2-isopropyl-4-methoxy-benzyl)-2-methylsulfanyl-pyrimidin-4-ylamine (0.504 g, 92%) as a white solid.

المصدر

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