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Ethyl chloroformate → HCID 20349084, 화합물

HRID 1449311
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HRID 1449311 반응식
[CH3:1][NH:2][C:3]([N:5]([C:7]1[CH:12]=[CH:11][C:10]([CH3:13])=[C:9]([N+:14]([O-:16])=[O:15])[CH:8]=1)O)=[O:4].[OH-].[Na+].Cl[C:20]([O:22]CC)=[O:21]>O1CCOCC1>[N+:14]([C:9]1[CH:8]=[C:7]([N:5]2[C:3](=[O:4])[N:2]([CH3:1])[C:20](=[O:21])[O:22]2)[CH:12]=[CH:11][C:10]=1[CH3:13])([O-:16])=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10928Ethyl chloroformateHCID 14798Sodium HydroxideHCID 20349075HCID 20349075, 화합물

생성물 1

HCID 20349084HCID 20349084, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

1-Methyl-3-(3'-nitro-4'-methylphenyl)-3-hydroxyurea (11 g; 0.049 mole) was dissolved in dioxane (80 ml.) and mixed with a 2 N aqueous sodium hydroxide (28.5 ml; 0.057 mole). Ethyl chloroformate (5.2 ml; 0.054 mole) was added dropwise at 10°-15° C. with stirring and the stirring continued for about 1/2 hour after the addition was completed. The product which precipitated as formed was removed by filtration, washed with water and dried. This product was recrystallized from methanol and dried under vacuum to yield 2-(3'-nitro-4'-methylphenyl)-4-methyl-1,2,4-oxadiazolidine-3,5-dione as yellow crystals melting 80°-81° C. and having the following elemental analysis as calculated for C10H9N3O5 :

후처리

  1. additionafter the addition
  2. customThe product which precipitated
  3. customas formed
  4. customwas removed by filtration
  5. washwashed with water
  6. customdried
  7. customThis product was recrystallized from methanol
  8. customdried under vacuum

출처 및 근거

ORD 기록
ord-0e3864c6585648e9b5c2d60a43e5589e
출처 데이터셋
uspto-grants-1980_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04190431

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