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

HRID 1650927ノート

反応式

HRID 1650927 の反応式
[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]

参加物

5

反応物 3

HCID 63651,1-DichloroethaneHCID 6595MethacrylamideHCID 65578Oxalyl chloride

生成物 1

HCID 137662253-Chloro-2-methylpropanoyl isocyanate

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒2 回

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-1d1aaef925914350a8c885d0d6004d21
出典データセット
uspto-grants-1990_05
特許番号
US04925982

反応ノート

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