Hydrochloric Acid → HCID 15631696、化合物

HRID 1721931ノート

反応式

HRID 1721931 の反応式
[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]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 14622775HCID 14622775、化合物

生成物 1

HCID 15631696HCID 15631696、化合物収率 61.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0baeb73ce5994df59d74fe1dfd42c0f6
出典データセット
uspto-grants-1989_08
特許番号
US04853404

反応ノート

読み込み中…