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Methanol → 1-Methyl-5-(methoxycarbonyl-methylene)-hydantoin

HRID 372164
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HRID 372164 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 11719MethylureaHCID 5459894Dimethylmaleate

생성물 1

HCID 542662761-Methyl-5-(methoxycarbonyl-methylene)-hydantoin

시약·촉매·용매 1

HCID 335O-Cresol용매

실험 절차

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.

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후처리

  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

출처 및 근거

ORD 기록
ord-45034e2b8cfd43faa420eb9f88703e39
출처 데이터셋
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04089860

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