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O-Xylene → HCID 178433617、化合物

HRID 1106250
ノート
印刷プレビュー

反応式

HRID 1106250 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 178433617HCID 178433617、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-7b46845f285841a28ed0369a24ca0a90
出典データセット
uspto-grants-1982_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04312870

反応ノート

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