Bromoacetic Acid → [2,3-Dichloro-4-(1-ethoxymethyl-5-pyrazolylcarbonyl)phenoxy]acetic acid

HRID 1721925ノート

反応式

HRID 1721925 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[C:6]([C:9]([C:11]2[N:15]([CH2:16][O:17][CH2:18][CH3:19])[N:14]=[CH:13][CH:12]=2)=[O:10])[CH:5]=[CH:4][C:3]=1[OH:20].Br[CH2:22][C:23]([OH:25])=[O:24].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Cl:1][C:2]1[C:7]([Cl:8])=[C:6]([C:9]([C:11]2[N:15]([CH2:16][O:17][CH2:18][CH3:19])[N:14]=[CH:13][CH:12]=2)=[O:10])[CH:5]=[CH:4][C:3]=1[O:20][CH2:22][C:23]([OH:25])=[O:24]

参加物

5

反応物 3

HCID 6227Bromoacetic AcidHCID 11430Potassium CarbonateHCID 14622774HCID 14622774、化合物

生成物 1

HCID 9864296[2,3-Dichloro-4-(1-ethoxymethyl-5-pyrazolylcarbonyl)phenoxy]acetic acid収率 56.3%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

0.63 g of 2,3-dichloro-4-(1-ethoxymethyl-5-pyrazolylcarbonyl)phenol, 0.58 g of bromoacetic acid and 1.11 g of potassium carbonate are added to 40 ml of acetone, and the mixture is refluxed for 48 hours. The reaction mixture is concentrated to remove solvent, and water is added to the residue. The aqueous mixture is washed with ethyl acetate, acidified with 10% hydrochloric acid and then extracted with ethyl acetate. The extract is washed with a saturated sodium chloride solution, dried and evaporated to remove solvent. The residue is crystallized with water, and the crystals are separated by filtration, washed successively with water and isopropyl ether, and dried to give 0.42 g of [2,3-dichloro-4-(1-ethoxymethyl-5-pyrazolylcarbonyl)phenoxy]acetic acid.

後処理

  1. temperaturethe mixture is refluxed for 48 hours
  2. concentrationThe reaction mixture is concentrated
  3. customto remove solvent, and water
  4. additionis added to the residue
  5. washThe aqueous mixture is washed with ethyl acetate
  6. extractionextracted with ethyl acetate
  7. washThe extract is washed with a saturated sodium chloride solution
  8. customdried
  9. customevaporated
  10. customto remove solvent
  11. customThe residue is crystallized with water
  12. customthe crystals are separated by filtration
  13. washwashed successively with water and isopropyl ether
  14. customdried

出典と根拠

ORDレコード
ord-bae290b93c5c434d85ea6ad0188b6633
出典データセット
uspto-grants-1989_08
特許番号
US04853404

反応ノート

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