Phosgene → 2-isocyanatoethyl acetate

HRID 1277745노트

반응식

HRID 1277745 반응식
[CH3:1][C:2]1[O:3][CH2:4][CH2:5][N:6]=1.[C:7](Cl)(Cl)=[O:8].[OH-:11].[Na+]>O.C(Cl)Cl>[C:2]([O:3][CH2:4][CH2:5][N:6]=[C:7]=[O:8])(=[O:11])[CH3:1]

참가 물질

6

반응물 3

HCID 6371PhosgeneHCID 14798Sodium HydroxideHCID 707132-Methyl-2-oxazoline

생성물 1

HCID 131350802-isocyanatoethyl acetate

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

In like manner, a 3-liter jacketed reaction vessel was charged with 288 ml of methylene chloride and cooled to 0° C. A solution of 2-methyl-2-oxazoline (77.5 g) in 137.7 ml of water, a solution of phosgene (131 g) in 280 ml of methylene chloride, and 250 ml of a 35 weight percent solution of aqueous sodium hydroxide were added simultaneously to the reaction vessel with cooling and stirring; the total additive time was approximately 55 minutes. Stirring was continued for 2 minutes after the addition was complete and the organic and aqueous layers then allowed to separate. The organic layer was isolated and dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The desired product was then obtained from the concentrated organic layer by distillation at 55°/5 mm Hg to give 74.8 g (65 percent of theory) of the desired product as a clear, colorless liquid. The product structure was likewise confirmed by infrared and nuclear magnetic resonance spectroscopy.

후처리

  1. customreaction vessel
  2. temperaturewith cooling
  3. stirringStirring
  4. waitwas continued for 2 minutes
  5. additionafter the addition
  6. customto separate
  7. customThe organic layer was isolated
  8. dry with materialdried over anhydrous sodium sulfate
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-509ed78033db42eea37174f8125777e2
출처 데이터셋
uspto-grants-1981_07
특허 번호
US04278809

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