MeOH tetrahydrofuran → Methyl 2-(methylsulfonyl)pyrimidine-4-carboxylate

HRID 2220931

반응식

HRID 2220931 반응식
O[O:2][S:3]([O-:5])=O.[K+].[CH3:7][O:8][C:9]([C:11]1[C:16](S)=[CH:15][N:14]=[C:13](C)[N:12]=1)=[O:10].CO.[CH2:21]1COCC1>>[CH3:7][O:8][C:9]([C:11]1[CH:16]=[CH:15][N:14]=[C:13]([S:3]([CH3:21])(=[O:5])=[O:2])[N:12]=1)=[O:10]

참가 물질

4

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 g, 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.

후처리

  1. customThe resulting suspension is partitioned between methylene chloride and water
  2. additionwith the addition of NaOH and re
  3. extractionextracted with solvent
  4. customThe combined organic layers are dried
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-22a2f92f0af34014a73156d256bde02c
출처 데이터셋
uspto-grants-2008_05
특허 번호
US07368455B2

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