Sulfuric Acid → Ethyl 2-[2-(3,5-dichlorophenyl)hydrazinylidene]propanoate

HRID 864520

反応式

HRID 864520 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][NH2:10])[CH:5]=[C:6]([Cl:8])[CH:7]=1.[C:11]([O:16][CH2:17][CH3:18])(=[O:15])[C:12]([CH3:14])=O.S(=O)(=O)(O)O.C(=O)(O)[O-].[Na+]>O.C(OCC)(=O)C.C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][N:10]=[C:12]([CH3:14])[C:11]([O:16][CH2:17][CH3:18])=[O:15])[CH:5]=[C:6]([Cl:8])[CH:7]=1

参加物

8

反応物 4

HCID 1118Sulfuric AcidHCID 12041Ethyl pyruvateHCID 516892Sodium BicarbonateHCID 6004693,5-Dichlorophenylhydrazine

生成物 1

HCID 71333082Ethyl 2-[2-(3,5-dichlorophenyl)hydrazinylidene]propanoate

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Combine 3,5-dichlorophenylhydrazine (300 g) and ethanol (2 L). Add ethyl pyruvate (153.6 mL) and sulfuric acid (25 mL). After 3 hours, evaporate in vacuo to obtain a residue. Cover the residue with ethyl acetate and water. Add solid sodium bicarbonate until the aqueous layer is neutralized. Separate the layers and extract the aqueous layer with ethyl acetate. Combine the organic layers, dry over MgSO4, filter, and evaporate in vacuo to give ethyl pyruvate-3,5-dichlorophenylhydrazone.

後処理

  1. customevaporate in vacuo
  2. customto obtain a residue
  3. customSeparate the layers
  4. extractionextract the aqueous layer with ethyl acetate
  5. dry with materialdry over MgSO4
  6. filtrationfilter
  7. customevaporate in vacuo

出典と根拠

ORDレコード
ord-2d1ace39198441088307ced858ae1bb0
出典データセット
uspto-grants-1996_10
特許番号
US05563157

関連ノート

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