Diethyl (ethoxymethylene)malonate → HCID 178469978, 화합물

HRID 443491

반응식

HRID 443491 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH:10][NH2:11])([O-:3])=[O:2].C([O:14][CH:15]=[C:16]([C:22](OCC)=O)[C:17]([O:19][CH2:20][CH3:21])=[O:18])C>C(O)C>[OH:14][C:15]1[N:10]([C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N+:1]([O-:3])=[O:2])[N:11]=[CH:22][C:16]=1[C:17]([O:19][CH2:20][CH3:21])=[O:18]

참가 물질

4

반응물 2

HCID 6871Diethyl (ethoxymethylene)malonateHCID 3314739(2-Nitrophenyl)hydrazine

생성물 1

HCID 178469978HCID 178469978, 화합물수율 43.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

102 g (2-nitrophenyl)hydrazine and 142 g (Ethoxymethylene)propanedioic acid, diethyl ester are dissolved in 300 ml ethanol and refluxed for 20 hours. After cooling the clear red solution is evaporated and the solvent distilled off. The remaining crystalline residue (168 g) is added to 400 g PPA (polyphosphoric acid) at a temperature of 80° C. The reaction is completed by heating the solution for 10 minutes to 120° C. The solution is then immediately poured on 2 kg ice and stirred for 30 minutes. After filtration the residue is recrystallized from n-propanol to yield 80 g of 5-hydroxy-1-(2-nitrophenyl)-1H-pyrazole-4-carboxylic acid, ethyl ester with a melting point of 157°-160° C.; yellow crystals.

후처리

  1. temperaturerefluxed for 20 hours
  2. temperatureAfter cooling the clear red solution
  3. customis evaporated
  4. distillationthe solvent distilled off
  5. additionThe remaining crystalline residue (168 g) is added to 400 g PPA (polyphosphoric acid) at a temperature of 80° C
  6. temperatureby heating the solution for 10 minutes to 120° C
  7. additionThe solution is then immediately poured on 2 kg ice
  8. filtrationAfter filtration the residue
  9. customis recrystallized from n-propanol

출처 및 근거

ORD 기록
ord-5bc60e2de038415b9acb005ffd3ccbf1
출처 데이터셋
uspto-grants-1981_04
특허 번호
US04260751

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