Hydrochloric Acid → HCID 15631696, 화합물

HRID 1721931노트

반응식

HRID 1721931 반응식
[Cl:1][C:2]1[C:14]([Cl:15])=[C:13]([C:16]([C:18]2[N:22](COCC)[N:21]=[CH:20][CH:19]=2)=[O:17])[CH:12]=[CH:11][C:3]=1[O:4][CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7].Cl.C(=O)(O)[O-].[Na+]>C(O)C>[Cl:1][C:2]1[C:14]([Cl:15])=[C:13]([C:16]([C:18]2[NH:22][N:21]=[CH:20][CH:19]=2)=[O:17])[CH:12]=[CH:11][C:3]=1[O:4][CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 14622775HCID 14622775, 화합물

생성물 1

HCID 15631696HCID 15631696, 화합물수율 61.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1.03 g of ethyl [2,3-dichloro-4-(1-ethoxymethyl-5-pyrazolylcarbonyl)phenoxy]acetate are dissolved in 25 ml of ethanol, and 6 ml of concentrated hydrochloric acid are added thereto. The mixture is stirred at 60°-65° C. for 3.5 hours. The reaction mixture is cooled, adjusted to pH 8-9 by addition of an aqueous saturated sodium bicarbonate solution under ice-cooling, and then extracted with ethyl acetate. The extract is washed successively with an aqueous saturated sodium bicarbonate solution and water, dried and evaporated to remove solvent. The residue is purified by silica gel column chromatography (solvent; benzene-ethyl acetate) and crystallized with a mixture of benzene and chloroform to give 0.54 g of ethyl [2,3-dichloro-4-(5-pyrazolylcarbonyl)phenoxy]acetate.

후처리

  1. temperatureThe reaction mixture is cooled
  2. temperaturecooling
  3. extractionextracted with ethyl acetate
  4. washThe extract is washed successively with an aqueous saturated sodium bicarbonate solution and water
  5. customdried
  6. customevaporated
  7. customto remove solvent
  8. customThe residue is purified by silica gel column chromatography (solvent; benzene-ethyl acetate)
  9. customcrystallized with a mixture of benzene and chloroform

출처 및 근거

ORD 기록
ord-0baeb73ce5994df59d74fe1dfd42c0f6
출처 데이터셋
uspto-grants-1989_08
특허 번호
US04853404

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