O-Cresol → HCID 54096441、化合物

HRID 372160

反応式

HRID 372160 の反応式
[CH3:1][NH:2][C:3]([NH:5][CH3:6])=[O:4].C/[C:8](/[C:14]([O-:16])=O)=[C:9](\C)/[C:10]([O-:12])=[O:11].[C:17]1(C)C(O)=CC=CC=1>ClC1C=CC=CC=1Cl>[CH3:1][N:2]1[C:8](=[CH:9][C:10]([O:12][CH3:17])=[O:11])[C:14](=[O:16])[N:5]([CH3:6])[C:3]1=[O:4]

参加物

5

反応物 3

HCID 335O-CresolHCID 7293N,N'-DimethylureaHCID 5459894Dimethylmaleate

生成物 1

HCID 54096441HCID 54096441、化合物

試薬・触媒・溶媒 1

HCID 72391,2-Dichlorobenzene溶媒

実験手順

44 g of N,N'-dimethylurea were dissolved in 150 g of o-dichlorobenzene and reacted with 72 g of dimethylmaleate for 2 hours at 180°-185° C after the addition of 25 g of cresol. The solvent was removed from this reaction mixture and the residue was fractionated under vacuum, 85 g (= 85% of the theory) of the desired product distilling over at 0.07 Torr and 128° C. A purified product melting at 49.5° C could be obtained by dissolving the crude product in chloroform and reprecipitating it with ether. The structure of the purified product was confirmed by IR and NMR spectra and by elementary analysis.

後処理

  1. customThe solvent was removed from this reaction mixture
  2. distillationdistilling over at 0.07 Torr and 128° C

出典と根拠

ORDレコード
ord-57af96b92cdb484db5e792ce9ad2d545
出典データセット
uspto-grants-1978_05
特許番号
US04089860

関連ノート

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