Methanol → Methyl 3-methoxy-2-(methoxymethyl)propanoate

HRID 1392744ノート

反応式

HRID 1392744 の反応式
[CH3:1][O-:2].[Na+].Br[CH2:5][C:6](=[CH2:11])[C:7]([O:9][CH3:10])=[O:8].[CH3:12][OH:13]>C(OCC)C>[CH3:1][O:2][CH2:5][CH:6]([CH2:11][O:13][CH3:12])[C:7]([O:9][CH3:10])=[O:8]

参加物

5

反応物 3

HCID 887MethanolHCID 5210932-Propenoic acid, 2-(bromomethyl)-, methyl esterHCID 10942334Sodium Methoxide

生成物 1

HCID 22934772Methyl 3-methoxy-2-(methoxymethyl)propanoate

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

Sodium methoxide (1.21 g) was added to a solution of methyl 2-(bromomethyl)acrylate (1.0 ml) in methanol (10 ml), and the mixture was heated under reflux for 26 hours. After cooling, the reaction mixture was diluted with diethyl ether, and precipitate was collected by filtration and the filtrate was concentrated under reduced pressure. The resultant residue was purified by column chromatography on silica gel (ethyl acetate:hexane=1:4) to obtain the title compound (726 mg).

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 26 hours
  3. temperatureAfter cooling
  4. filtrationwas collected by filtration
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe resultant residue was purified by column chromatography on silica gel (ethyl acetate:hexane=1:4)

出典と根拠

ORDレコード
ord-61a4ad58fd024dc1af01e08dffb50109
出典データセット
uspto-grants-2008_03
特許番号
US07342014B2

反応ノート

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