Chloroform → 2,3-Dichloropropanoyl isocyanate

HRID 866774ノート

反応式

HRID 866774 の反応式
ClCl.[C:3]([NH2:7])(=[O:6])C=C.[C:8]([Cl:13])(=O)[C:9](Cl)=[O:10].[CH:14]([Cl:17])(Cl)Cl>>[Cl:13][CH:8]([CH2:14][Cl:17])[C:9]([N:7]=[C:3]=[O:6])=[O:10]

参加物

5

反応物 4

HCID 6212ChloroformHCID 6579AcrylamideHCID 24526ChlorineHCID 65578Oxalyl chloride

生成物 1

HCID 203185352,3-Dichloropropanoyl isocyanate収率 72%

実験手順

99 g (1.40 moles) of chlorine were passed into a solution of 100 g (1.41 moles) of acrylamide in 1,000 ml of chloroform while stirring at about 0° to 5° C. The mixture was then stirred for a further 3 hours at about 20° C, after which 270 g (2.13 moles) of oxalyl chloride was added dropwise, while continuing the stirring. The solution was then heated to the boil under reflux, until the evolution of gas had ceased. Fractional distillation of the reaction solution gave 172 g (72% theory) of 2,3-dichloro-propionyl isocyanate of boiling point 38 to 41° C/1.0 mm Hg. ##STR76##

後処理

  1. stirringThe mixture was then stirred for a further 3 hours at about 20° C
  2. temperatureThe solution was then heated to the boil
  3. temperatureunder reflux, until the evolution of gas
  4. distillationFractional distillation of the reaction solution

出典と根拠

ORDレコード
ord-b3ce25167c8b4ae0836369995793202e
出典データセット
uspto-grants-1978_07
特許番号
US04101575

反応ノート

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