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Sodium Thiosulfate → HCID 14622781、化合物

HRID 1721933
ノート
印刷プレビュー

反応式

HRID 1721933 の反応式
[Cl:1][O-].[Na+].[Cl:4][C:5]1[C:15]([Cl:16])=[C:14]([C:17]([C:19]2[N:23]([CH2:24][CH3:25])[N:22]=[CH:21][CH:20]=2)=[O:18])[CH:13]=[CH:12][C:6]=1[O:7][CH2:8][C:9]([OH:11])=[O:10].S([O-])([O-])(=O)=S.[Na+].[Na+]>C(O)(=O)C.CN(C)C=O.O>[Cl:4][C:5]1[C:15]([Cl:16])=[C:14]([C:17]([C:19]2[N:23]([CH2:24][CH3:25])[N:22]=[CH:21][C:20]=2[Cl:1])=[O:18])[CH:13]=[CH:12][C:6]=1[O:7][CH2:8][C:9]([OH:11])=[O:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 24477Sodium ThiosulfateHCID 14721234[2,3-Dichloro-4-(1-ethyl-1H-pyrazole-5-carbonyl)phenoxy]acetic acidHCID 23665760Sodium Hypochlorite2 回

生成物 1

HCID 14622781HCID 14622781、化合物

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 962Water
溶媒
HCID 6228Dimethylformamide溶媒

実験手順

6.7 g of an aqueous 10% sodium hypochlorite solution are added dropwise to a solution of 2.36 g of [2,3-dichloro-4-(1-ethyl-5-pyrazolylcarbonyl)phenoxy]acetic acid in a mixture of 50 ml of acetic acid and 20 ml of dimethylformamide, and the mixture is stirred at room temperature for 30 minutes. A solution of 2.0 g of sodium thiosulfate in 5 ml of water is added to the reaction mixture to decompose excess sodium hypochloride, and the mixture is evaporated to remove solvent. The residue (oil) is dissolved in water, and the solution is adjusted to pH 3 with 1N hydrochloric acid and extracted with ethyl acetate. The extract is washed with water, dried and evaporated to remove solvent. The residue is crystallized from a mixture of ethyl acetate and hexane to give 2.19 g of [2,3-dichloro-4-(4-chloro-1-ethyl-5-pyrazolylcarbonyl)phenoxy]acetic acid.

後処理

  1. customthe mixture is evaporated
  2. customto remove solvent
  3. dissolutionThe residue (oil) is dissolved in water
  4. extractionextracted with ethyl acetate
  5. washThe extract is washed with water
  6. customdried
  7. customevaporated
  8. customto remove solvent
  9. customThe residue is crystallized from a mixture of ethyl acetate and hexane

出典と根拠

ORDレコード
ord-e698ab07a66641908d2951c0436ed5e9
出典データセット
uspto-grants-1989_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04853404

反応ノート

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