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

HRID 1602363

반응식

HRID 1602363 반응식
[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

참가 물질

8

반응물 4

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

생성물 1

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

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-010acf663e2d44aa8dbe736c872f676f
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05981553

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