Methanol → HCID 54266276、化合物

HRID 372164

反応式

HRID 372164 の反応式
C/[C:2](/[C:8]([O-:10])=O)=[C:3](\C)/[C:4]([O-:6])=[O:5].[CH3:11]O.[CH3:13][NH:14][C:15]([NH2:17])=[O:16]>C1(C)C(O)=CC=CC=1>[CH3:13][N:14]1[C:2](=[CH:3][C:4]([O:6][CH3:11])=[O:5])[C:8](=[O:10])[NH:17][C:15]1=[O:16]

参加物

5

反応物 3

HCID 887MethanolHCID 11719MethylureaHCID 5459894Dimethylmaleate

生成物 1

HCID 54266276HCID 54266276、化合物

試薬・触媒・溶媒 1

HCID 335O-Cresol溶媒

実験手順

Proceeding in a similar manner to Example 3, 222 g of methyl urea were dissolved in 1000 g of cresol, and 432 g of dimethylmaleate were added. After termination of the reaction during which 92 g of methanol were liberated, and after gas chromatographic analysis showed 95% conversion of the reactants, the cresol was distilled off and the residue fractionated under vacuum. The main fraction distilling over at 140° to 143° C/0.06 Torr was recrystallised from ethyl acetate. The identity of the pure substance obtained, which melted at 100° C, could be confirmed by the IR and NMR spectra and elementary analysis.

後処理

  1. distillationthe cresol was distilled off
  2. distillationThe main fraction distilling over at 140° to 143° C/0.06 Torr
  3. customwas recrystallised from ethyl acetate
  4. customThe identity of the pure substance obtained

出典と根拠

ORDレコード
ord-45034e2b8cfd43faa420eb9f88703e39
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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