1,1-Dichloroethane → 3-Chloro-2-methylpropanoyl isocyanate

HRID 1650927노트

반응식

HRID 1650927 반응식
[C:1]([NH2:6])(=[O:5])[C:2]([CH3:4])=[CH2:3].C(Cl)(=O)[C:8](Cl)=[O:9].[Cl:13]C(Cl)C>Cl>[CH3:3][CH:2]([CH2:4][Cl:13])[C:1]([N:6]=[C:8]=[O:9])=[O:5]

참가 물질

5

반응물 3

HCID 63651,1-DichloroethaneHCID 6595MethacrylamideHCID 65578Oxalyl chloride

생성물 1

HCID 137662253-Chloro-2-methylpropanoyl isocyanate

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매2회

실험 절차

Into a suspension of methacrylamide (106 g; 1.25 mol) in dichloroethane (600 ml), dry hydrogen chloride gas was blown while cooling with ice for about 1 hour. Then, oxalyl chloride (243.9 g; 1.92 mol) was dropwise added thereto while continuing hydrogen chloride blowing and ice cooling. The resultant mixture was heated to reflux, and the refluxing was continued for 30 minutes. After being allowed to cool, the reaction mixture was distilled under reduced pressure to give alpha-methyl-beta-chloropropionyl isocyanate.

후처리

  1. temperaturewhile cooling with ice for about 1 hour
  2. temperatureto reflux
  3. temperatureto cool
  4. distillationthe reaction mixture was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-1d1aaef925914350a8c885d0d6004d21
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04925982

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