Acetone → HCID 57419464、化合物

HRID 1962319

反応式

HRID 1962319 の反応式
O[C:2]1[C:10]([I:11])=[CH:9][C:8]([I:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S([O:18][CH3:19])(OC)(=O)=O.[CH3:20]C(C)=O>>[I:11][C:10]1[C:2]([O:18][CH3:19])=[C:3]([CH:7]=[C:8]([I:12])[CH:9]=1)[C:4]([O:6][CH3:20])=[O:5]

参加物

4

反応物 3

HCID 180AcetoneHCID 6497Dimethyl SulfateHCID 86313,5-Diiodosalicylic acid

生成物 1

HCID 57419464HCID 57419464、化合物

実験手順

A mixture of 2-hydroxy-3,5-diiodobenzoic acid (3.9 g, 10.0 mmol) potassium carbonate (4.15 g, 30.0 mmol) and dimethyl sulfate (2.77 g, 22.0 mmol) in acetone (33 ml) was heated at reflux for 16 h, cooled and concentrated. The residue was dissolved in EtOAc and washed with water, brine, dried (Na2SO4), filtered and concentrated to give an off-white solid (4.2 g, quantitative yield).

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 16 h
  3. temperaturecooled
  4. concentrationconcentrated
  5. dissolutionThe residue was dissolved in EtOAc
  6. washwashed with water, brine
  7. dry with materialdried (Na2SO4)
  8. filtrationfiltered
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-f2eee1525b204e288b52bcb181a85185
出典データセット
uspto-grants-2013_04
特許番号
US08415351B2

関連ノート

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