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1-Propanol → 3-(4-Iodophenyl)-1-(4-cyanophenyl)-4-ethoxycarbonyl-2-methyl-2H-pyrazol-5-one

HRID 1740084
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HRID 1740084 반응식
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([NH:9][NH:10][CH3:11])=[CH:5][CH:4]=1)#[N:2].[I:12][C:13]1[CH:18]=[CH:17][C:16]([C:19](Cl)=[C:20]([C:26]([O:28]CC)=O)[C:21]([O:23][CH2:24][CH3:25])=[O:22])=[CH:15][CH:14]=1.C(N(C(C)C)CC)(C)C.C(O)CC>C(OCC)(=O)C>[I:12][C:13]1[CH:14]=[CH:15][C:16]([C:19]2[N:10]([CH3:11])[N:9]([C:6]3[CH:5]=[CH:4][C:3]([C:1]#[N:2])=[CH:8][CH:7]=3)[C:26](=[O:28])[C:20]=2[C:21]([O:23][CH2:24][CH3:25])=[O:22])=[CH:17][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 10311-PropanolHCID 81531DiisopropylethylamineHCID 21837631Ethyl 3-(4-iodophenyl)-3-chloro-2-ethoxycarbonylacrylateHCID 218376391-(4-Cyanophenyl)-2-methylhydrazine

생성물 1

HCID 218376333-(4-Iodophenyl)-1-(4-cyanophenyl)-4-ethoxycarbonyl-2-methyl-2H-pyrazol-5-one수율 55.9%

시약·촉매·용매 1

HCID 8857
Ethyl Acetate
용매

실험 절차

A mixture of 29.34 g of 1-(4-cyanophenyl)-2-methylhydrazine, 65.17 g of ethyl 3-(4-iodophenyl)-3-chloro-2-ethoxycarbonylacrylate, 30.9 g of diisopropylethylamine and 300 ml of 1-propanol was refluxed under heating for 17 hours, then cooled and stirred with 200 ml of ethyl acetate at room temperature for 20 hours. The precipitated crystals were collected by filtration and washed with hexane-ethyl acetate to give 42.21 g of the title compound as pale yellow crystals.

후처리

  1. temperaturewas refluxed
  2. temperatureunder heating for 17 hours
  3. temperaturecooled
  4. filtrationThe precipitated crystals were collected by filtration
  5. washwashed with hexane-ethyl acetate

출처 및 근거

ORD 기록
ord-3734deefe61c458d894b3070703105b0
출처 데이터셋
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05968967

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