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Hydrochloric Acid → 3-Methoxy-2,4-dioxoimidazolidine

HRID 236543
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HRID 236543 반응식
[CH3:1][O:2][NH3+:3].[Cl-].[OH-].[K+].[N:7]([CH2:10][C:11](OCC)=[O:12])=[C:8]=[O:9].Cl>O>[CH3:1][O:2][N:3]1[C:11](=[O:12])[CH2:10][NH:7][C:8]1=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 11639O-methylhydroxylammonium chlorideHCID 14797Potassium HydroxideHCID 76283Ethyl isocyanatoacetate

생성물 1

HCID 138225763-Methoxy-2,4-dioxoimidazolidine수율 69.2%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

An aqueous solution prepared by dissolving 3.34 g of hydroxylamine methyl ether hydrochloride in 20 ml of water, was cooled with ice. While stirring the solution, an aqueous solution prepared by dissolving 2.24 g of potassium hydroxide in 20 ml of water, was gradually dropwise added thereto. After completion of the dropwise addition, the reaction system was returned to room temperature and the stirring was continued for 1 hour. Then, the reaction mixture was again cooled with ice, and 2.58 g of ethyl isocyanatoacetate was gradually added. The reaction system was returned to room temperature, and the reaction solution was stirred at a temperature of from 40° to 50° C. for further 0.5 hour. Then, the reaction solution was cooled with ice, and 10 ml of 6N hydrochloric acid was added. The mixture was refluxed for 3 hours, and then cooled with ice, whereby crystals precipitated. The crystals were collected by filtration to obtain 1.8 g of 3-methoxy-2,4-dioxoimidazolidine having a melting point of from 98° to 107° C.

후처리

  1. customAn aqueous solution prepared
  2. temperaturewas cooled with ice
  3. customan aqueous solution prepared
  4. additionwas gradually dropwise added
  5. additionAfter completion of the dropwise addition
  6. customwas returned to room temperature
  7. additionwas gradually added
  8. customwas returned to room temperature
  9. stirringthe reaction solution was stirred at a temperature of from 40° to 50° C. for further 0.5 hour
  10. additionwas added
  11. temperatureThe mixture was refluxed for 3 hours
  12. temperaturecooled with ice, whereby crystals
  13. customprecipitated
  14. filtrationThe crystals were collected by filtration

출처 및 근거

ORD 기록
ord-93c9995a83544e3dad523c2084b028c0
출처 데이터셋
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04645761

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