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

HRID 1721925노트

반응식

HRID 1721925 반응식
[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]

참가 물질

5

반응물 3

HCID 6227Bromoacetic AcidHCID 11430Potassium CarbonateHCID 14622774HCID 14622774, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bae290b93c5c434d85ea6ad0188b6633
출처 데이터셋
uspto-grants-1989_08
특허 번호
US04853404

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