Iodoacetic Acid → HCID 13958742、化合物

HRID 255943

反応式

HRID 255943 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[C:6]([C:9](=[O:12])[CH:10]=[CH2:11])[CH:5]=[CH:4][C:3]=1[OH:13].I[CH2:15][C:16]([OH:18])=[O:17].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Cl:1][C:2]1[C:7]([Cl:8])=[C:6]([C:9](=[O:12])[CH:10]=[CH2:11])[CH:5]=[CH:4][C:3]=1[O:13][CH2:15][C:16]([OH:18])=[O:17]

参加物

5

反応物 3

HCID 5240Iodoacetic AcidHCID 11430Potassium CarbonateHCID 13958744HCID 13958744、化合物

生成物 1

HCID 13958742HCID 13958742、化合物収率 35.7%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

2,3-Dichloro-4-acryloylphenol (4.85 g, 0.0224 mole), iodoacetic acid (4.5 g, 0.24 mole), potassium carbonate (3.33 g, 0.024 mole) and acetone (200 ml) were united, stirred and refluxed for 20 hours. The reaction mixture was cooled and the solid removed by filtration, dissolved in water (100 ml) and acidified to a pH of 1 with concentrated hydrochloric acid. The material that separated was extracted with chloroform, the organic layer removed, washed with water, dried over MgSO4, filtered and the solvent removed by evaporation in vacuo. The residue was recrystallized from carbon tetrachloride to give 2.2 g of (2,3-dichloro-4-acryloylphenoxy)-acetic acid, m.p. 111°-113° C.

後処理

  1. temperaturerefluxed for 20 hours
  2. temperatureThe reaction mixture was cooled
  3. customthe solid removed by filtration
  4. dissolutiondissolved in water (100 ml)
  5. customThe material that separated
  6. extractionwas extracted with chloroform
  7. customthe organic layer removed
  8. washwashed with water
  9. dry with materialdried over MgSO4
  10. filtrationfiltered
  11. customthe solvent removed by evaporation in vacuo
  12. customThe residue was recrystallized from carbon tetrachloride

出典と根拠

ORDレコード
ord-e78cce5e0b18492bb04bdc49b63ef128
出典データセット
uspto-grants-1987_10
特許番号
US04699926

関連ノート

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