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Methacrylamide → Ethyl [(2-methylacryloyl)amino](oxo)acetate

HRID 1073657
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HRID 1073657 반응식
[C:1]([NH2:6])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:7](Cl)([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:8]>C1C=CC=CC=1>[C:7]([NH:6][C:1](=[O:5])[C:2]([CH3:4])=[CH2:3])([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:8]
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참가 물질

4

반응물 2

HCID 6595MethacrylamideHCID 20884Ethoxalyl chloride

생성물 1

HCID 14298183Ethyl [(2-methylacryloyl)amino](oxo)acetate수율 42.9%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

Into a reaction vessel equipped with a stirrer, a cooler, an nitrogen gas introducing inlet and a dropping funnel, benzene (288.5 ml) and methacrylamide (49.1 g; 0.577 mol) were charged, and the resulting mixture was heated with reflux. Refluxing and bubbling with nitrogen gas were continued, during which ethoxalyl chloride (78.5 g; 0.577 mol) was dropwise added thereto in 2.5 hours. After the dropwise addition was completed, refluxing was continued for 5 hours. The benzene was distilled off, hydroquinone (0.01 g) was added thereto, and distillation under reduced pressure was carried out to give N-ethoxalylmethacrylamide (45.8 g). Yield, 43%. B.P., 110-115° C./0.3 mmHg. Refractive index, 1.473.

후처리

  1. customInto a reaction vessel equipped with a stirrer
  2. additiona cooler, an nitrogen gas introducing inlet and a dropping funnel
  3. temperaturethe resulting mixture was heated
  4. temperaturewith reflux
  5. temperatureRefluxing
  6. custombubbling with nitrogen gas
  7. additionwas dropwise added
  8. additionAfter the dropwise addition
  9. temperaturerefluxing
  10. waitwas continued for 5 hours
  11. distillationThe benzene was distilled off
  12. additionhydroquinone (0.01 g) was added
  13. distillationdistillation under reduced pressure

출처 및 근거

ORD 기록
ord-95395c1ff753489589c39cfe63252450
출처 데이터셋
uspto-grants-1990_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04970281

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