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O-Xylene → HCID 178433617, 화합물

HRID 1106250
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HRID 1106250 반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]([CH3:12])[C:3]=1[C:13]([O:15]CC)=O.[C:18]1([NH:24][NH2:25])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C1(C)C(C)=CC=CC=1>C(OCC)C>[CH3:12][C:4]1[NH:5][C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:11]=2[C:2]2[C:3]=1[C:13](=[O:15])[N:24]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[N:25]=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7237O-XyleneHCID 7516PhenylhydrazineHCID 105386043-Quinolinecarboxylic acid, 4-chloro-2-methyl-, ethyl ester

생성물 1

HCID 178433617HCID 178433617, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

The mixture of 3.6 g of ethyl 4-chloro-2-methylquinolin-3-carboxylate, 1.8 g of phenylhydrazine and 40 ml of xylene is refluxed for 4 hours, cooled to room temperature, diluted with diethyl ether and filtered. The residue is dissolved in 50 ml of 2 N aqueous sodium hydroxide, the solution washed with diethyl ether and its pH adjusted to 8.5 with ammonium chloride. The precipitate formed is collected, washed successively with hot water, methanol and diethyl ether, to yield the 4-methyl-2-phenylpyrazolo[4,3-c]quinolin-3(5H)-one, showing in the IR-spectrum peaks at 874, 867, 858, 850, 822, 780, 765, 756, 750, 740 and 722 cm-1. Analogously the 4-methyl-2-(p-chlorophenyl)-pyrazolo[4-3,-c]quinolin-3(5H)-one is prepared, melting at 349°-350°.

후처리

  1. temperatureis refluxed for 4 hours
  2. filtrationfiltered
  3. dissolutionThe residue is dissolved in 50 ml of 2 N aqueous sodium hydroxide
  4. washthe solution washed with diethyl ether and its pH
  5. customThe precipitate formed
  6. customis collected
  7. washwashed successively with hot water, methanol and diethyl ether

출처 및 근거

ORD 기록
ord-7b46845f285841a28ed0369a24ca0a90
출처 데이터셋
uspto-grants-1982_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04312870

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