Potassium Carbonate → 6-Methoxy-4-{2-[(2R)-oxiran-2-yl]ethyl}pyrido[2,3-b]pyrazin-3(4H)-one

HRID 1847072ノート

反応式

HRID 1847072 の反応式
CC1C=CC(S(O[CH2:12][C@H:13]([OH:29])[CH2:14][CH2:15][N:16]2[C:21](=[O:22])[CH:20]=[N:19][C:18]3[CH:23]=[CH:24][C:25]([O:27][CH3:28])=[N:26][C:17]2=3)(=O)=O)=CC=1.C(=O)([O-])[O-].[K+].[K+]>CO>[CH3:28][O:27][C:25]1[CH:24]=[CH:23][C:18]2[N:19]=[CH:20][C:21](=[O:22])[N:16]([CH2:15][CH2:14][C@@H:13]3[CH2:12][O:29]3)[C:17]=2[N:26]=1

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 86724995(2R)-2-Hydroxy-4-(6-methoxy-3-oxopyrido[2,3-b]pyrazin-4(3H)-yl)butyl 4-methylbenzensulfonate

生成物 1

HCID 867249966-Methoxy-4-{2-[(2R)-oxiran-2-yl]ethyl}pyrido[2,3-b]pyrazin-3(4H)-one

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In methanol (250 ml) was dissolved (2R)-2-hydroxy-4-(6-methoxy-3-oxopyrido[2,3-b]pyrazin-4(3H)-yl)butyl 4-methylbenzensulfonate (4.30 g, 10.25 mmol), potassium carbonate (1.70 g, 12.30 mmol) was added thereto at room temperature and the mixture was stirred for 4 hours. The reaction solution was concentrated under reduced pressure and the residue was diluted with chloroform and washed with water. After drying the resultant over anhydrous sodium sulfate, the solvent was removed under reduced pressure and the obtained residue was purified by silica gel column chromatography (chloroform/methanol) to yield 2.62 g (quantitative) of the title compound in the form of a yellowish solid.

後処理

  1. additionwas added
  2. concentrationThe reaction solution was concentrated under reduced pressure
  3. additionthe residue was diluted with chloroform
  4. washwashed with water
  5. dry with materialAfter drying the resultant over anhydrous sodium sulfate
  6. customthe solvent was removed under reduced pressure
  7. customthe obtained residue was purified by silica gel column chromatography (chloroform/methanol)

出典と根拠

ORDレコード
ord-3332704ccac542afbf11c8b374062ae0
出典データセット
uspto-grants-2015_02
特許番号
US08952010B2

反応ノート

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