Acetone → HCID 57419464、化合物

HRID 2280599

反応式

HRID 2280599 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-cfbddf66c38f4181be7b0e49b7c128a7
出典データセット
uspto-grants-2015_09
特許番号
US09139536B2

関連ノート

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