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Methanol → Methyl 5-(benzyloxy)-1-methyl-2-(methylsulfonyl)-6-oxo-1,6-dihydropyrimidine-4-carboxylate

HRID 1409588
ノート
印刷プレビュー

反応式

HRID 1409588 の反応式
[CH2:1]([O:8][C:9]1[C:14](=[O:15])[N:13]([CH3:16])[C:12](SC)=[N:11][C:10]=1[C:19]([O:21][CH3:22])=[O:20])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:23]O.C(Cl)Cl.O[O:29][S:30]([O-:32])=O.[K+]>O>[CH3:22][O:21][C:19]([C:10]1[N:11]=[C:12]([S:30]([CH3:23])(=[O:32])=[O:29])[N:13]([CH3:16])[C:14](=[O:15])[C:9]=1[O:8][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)=[O:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 887MethanolHCID 6344DichloromethaneHCID 23707502Potassium hydroxy sulfiteHCID 86710286Methyl 5-(benzyloxy)-1-methyl-2-(methylthio)-6-oxo-1,6-dihydropyrimidine-4-carboxylate

生成物 1

HCID 86710287Methyl 5-(benzyloxy)-1-methyl-2-(methylsulfonyl)-6-oxo-1,6-dihydropyrimidine-4-carboxylate収率 60%

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

実験手順

In a 1 L round-bottomed flask, methyl 5-(benzyloxy)-1-methyl-2-(methylthio)-6-oxo-1,6-dihydropyrimidine-4-carboxylate (5.57 g, 17.4 mmol) was combined with MeOH (400 ml) and DCM (50 ml). A solution of oxone (21.4 g, 34.8 mmol) in water (100 ml) was added. The mixture was stirred at room temperature for 5 hours and then evaporated to dryness. The residue was taken up into EtOAc, washed with 3N NaOH aqueous solution, water, and brine, dried over Na2SO4 and concentrated under reduced pressure to give the title compound as a white solid (3.7 g; 60%). LCMS: m/z=353 (MH+).

後処理

  1. customevaporated to dryness
  2. washwashed with 3N NaOH aqueous solution, water, and brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-da95aed1b9394042bacf66be36652d97
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08921388B2

反応ノート

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