Chloroform → 2,3-Dichloropropanoyl isocyanate

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

反応物 4

HCID 6212Chloroform

HCID 6579Acrylamide

HCID 24526Chlorine

HCID 65578Oxalyl chloride

生成物 1

HCID 203185352,3-Dichloropropanoyl isocyanate

反応条件

温度: 20 °C

実験手順

99 g (1.40 mol) of chlorine are introduced with stirring at about 0 to 5° C. into a solution of 100 g of acrylic acid amide in 1000 ml of chloroform. After stirring for 3 hours at about 20° C., 270 g (2.13 mol) of oxalyl chloride are added dropwise with continued stirring. The solution is then boiled under reflux until the evolution of gas is complete. Fractional distillation of the reaction solution gives 172 g (72 % of the theoretical amount) of 2,3-dichloropropionyl isocyanate boiling at 38 to 41° C./1.0 Torr.

後処理

temperatureunder reflux until the evolution of gas
distillationFractional distillation of the reaction solution

出典と根拠

ORDレコード: ord-1b2027bcf7c744eca3cc26229f213ca9
出典データセット: uspto-grants-1977_07
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US04036850

反応ノート

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