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

HRID 1032074
ノート
印刷プレビュー

反応式

HRID 1032074 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6595MethacrylamideHCID 20884Ethoxalyl chloride

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b7f30c54e2cc44a798c966b45b60c106
出典データセット
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04956491

反応ノート

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