Methanol → methyl (Z)-3-(3-butoxy-4-iodophenyl)-2-ethoxyacrylate

HRID 390631ノート

反応式

HRID 390631 の反応式
[CH2:1]([O:5][C:6]1[CH:7]=[C:8](/[CH:13]=[C:14](\[O:18][CH2:19][CH3:20])/[C:15]([OH:17])=[O:16])[CH:9]=[CH:10][C:11]=1[I:12])[CH2:2][CH2:3][CH3:4].S(=O)(=O)(O)O.O.[CH3:27]O>>[CH2:1]([O:5][C:6]1[CH:7]=[C:8](/[CH:13]=[C:14](\[O:18][CH2:19][CH3:20])/[C:15]([O:17][CH3:27])=[O:16])[CH:9]=[CH:10][C:11]=1[I:12])[CH2:2][CH2:3][CH3:4]

参加物

5

反応物 4

HCID 887MethanolHCID 962WaterHCID 1118Sulfuric AcidHCID 68961569(Z)-3-(3-butoxy-4-iodophenyl)-2-ethoxyacrylic acid

生成物 1

HCID 86626090methyl (Z)-3-(3-butoxy-4-iodophenyl)-2-ethoxyacrylate収率 61%

実験手順

In an Emrys Optimizer microwave reactor, 0.8 g (2 mmol) of (Z)-3-(3-butoxy-4-iodophenyl)-2-ethoxyacrylic acid is dissolved in 10 mL of methanol and 1 mL of concentrated sulfuric acid and heated at 70° C. by microwave for 2 hours. After addition of water, the reaction medium is extracted with ethyl acetate. The organic phase is washed with water, dried over magnesium sulfate, filtered and evaporated. 0.5 g (61%) of methyl (Z)-3-(3-butoxy-4-iodophenyl)-2-ethoxyacrylate is obtained.

後処理

  1. extractionthe reaction medium is extracted with ethyl acetate
  2. washThe organic phase is washed with water
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated

出典と根拠

ORDレコード
ord-b4d3a86657794a0c8da4344e60d494dc
出典データセット
uspto-grants-2013_02
特許番号
US08383652B2

反応ノート

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