Potassium Carbonate → Methyl 2-hydroxy-3-methylbutanoate

HRID 847116

反応式

HRID 847116 の反応式
[CH3:1][C:2]1[CH:7]=C(C)N=C(S(C)(=O)=O)N=1.C(=O)([O-])[O-:14].[K+].[K+].[C:19]([O:22][CH2:23]C)(=[O:21])[CH3:20].CCCCCC>CC(C)=O>[OH:14][CH:20]([CH:2]([CH3:7])[CH3:1])[C:19]([O:22][CH3:23])=[O:21]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 27723824,6-Dimethyl-2-methylsulfonylpyrimidineHCID 21226206Ethyl acetate hexane

生成物 1

HCID 552631Methyl 2-hydroxy-3-methylbutanoate収率 42%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

1.5g of the product of (b) and 2.llg (0.011 moles) of 4,6-dimethyl-2-methanesulphonyl pyrimidine were dissolved in 20ml acetone. 1.6g of potassium carbonate were added and the reaction mixture refluxed for 4 hours. Following thin layer chromatography to establish that the reaction had reached completion, the mixture was evaporated to dryness and 10ml water added. Solvent extraction using chloroform followed and the chloroform extracts were dried over anhydrous sodium sulphate and the solvent evaporated off. The oil resulting was subjected to flash column chromatography using ethyl acetate: hexane (1:1) as eluant to yield 1.1g (yield 42%) of the title compound as a colourless oil.

後処理

  1. temperaturethe reaction mixture refluxed for 4 hours
  2. customthe mixture was evaporated to dryness and 10ml water
  3. additionadded
  4. extractionSolvent extraction
  5. dry with materialthe chloroform extracts were dried over anhydrous sodium sulphate
  6. customthe solvent evaporated off
  7. customThe oil resulting

出典と根拠

ORDレコード
ord-cf79931c56a949f79b58fb9cfb194278
出典データセット
uspto-grants-1992_08
特許番号
US05139563

関連ノート

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