تفاعل #86502

ord-a1a37df2a7c047c4a48b07db83119876

المذيبات

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAfter removal of acetonitrile in vacuum
  2. 2
    workup.DISSOLUTIONthe resulting solid was dissolved in methylene chloride
  3. 3
    غسيلwashed with water, saturated Na2S2O3, saturated sodium bicarbonate, and brine
  4. 4
    تجفيفand then the organic layers dried over sodium sulfate
  5. 5
    ترشيحfiltered
  6. 6
    تركيزThe filtrate was concentrated under reduced pressure

الإجراء التجريبي

A mixture of 2-(1-bromopropyl)-6-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (3.46 g, 12.3 mmol) and N-iodosuccinimide (4.15 g, 18.4 mmol) in acetonitrile (100 mL) was stirred at 80° C., under nitrogen, overnight. After removal of acetonitrile in vacuum, the resulting solid was dissolved in methylene chloride, washed with water, saturated Na2S2O3, saturated sodium bicarbonate, and brine; and then the organic layers dried over sodium sulfate and then filtered. The filtrate was concentrated under reduced pressure to provide the desired product (4.53 g, 90.4%). LCMS calculated for C12H13BrIN2O (M+H)+: m/z=406.9. Found: 407.1.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09434746B2uspto-grants-2016_09