반응 #7741

ord-dead07a44f7a4bb99af3704ce3bf4d5d

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The resulting suspension is partitioned between methylene chloride and water
  2. 2
    workup.ADDITIONwith the addition of NaOH and re
  3. 3
    추출extracted with solvent
  4. 4
    기타The combined organic layers are dried
  5. 5
    여과filtered
  6. 6
    농축concentrated in vacuo

실험 절차

An aqueous solution (1 L) of Oxone® (211.7 g, 344 mmol) is added dropwise at 0° C. to a solution of 2-methyl-sulfanyl-pyrimidine-4-carboxylic acid methyl ester, 14, (19 9,86.1 mmol) in 1:1 methanol/THF (1 L). The reaction solution is allowed to warm to room temperature and stir for 1.5 hours. The resulting suspension is partitioned between methylene chloride and water. The aqueous phase is made alkaline with the addition of NaOH and re extracted with solvent. The combined organic layers are dried, filtered, and concentrated in vacuo to afford 18.4 g of the desired product as a yellow oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07087615B2uspto-grants-2006_08