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硝酸铽(III)水合物 → Propane, 1,2-dichloro-2-fluoro-3-nitro-

HRID 893406
笔记
打印预览

反应方程式

HRID 893406 反应方程式
[N+:1]([O-:4])(O)=[O:2].[Cl:5][C:6]([CH2:8][Cl:9])=[CH2:7].[FH:10]>>[Cl:5][C:6]([F:10])([CH2:8][Cl:9])[CH2:7][N+:1]([O-:4])=[O:2]
参与物实验过程后处理来源与证据反应笔记

参与物

4

反应物 3

HCID 944硝酸铽(III)水合物HCID 65652,3-二氯丙烯HCID 14917氢氟酸

产物 1

HCID 10954045Propane, 1,2-dichloro-2-fluoro-3-nitro-

实验过程

To a mixture of 86 ml of anhydrous, 100% strength nitric acid and 300 ml of anhydrous hydrofluoric acid were added dropwise at -10° C. in the course of 3 hours 111 g (1 mol) of 2,3-dichloropropene. The reaction was slightly exothermic. After the dropwise addition had ceased, stirring was continued for a further 1 hour at -10° C. Then the mixture was poured on to ice and extracted using dichloromethane. The organic phase was washed with sodium hydrogencarbonate solution, dried over sodium sulphate and concentrated using a rotary evaporator. The crude product was distilled under an oil pump vacuum. This gave 115.8 g (=63% of theory) of product having a boiling point of 48° to 50° C. at 0.07 mbar and a Refractive Index nD20 of 1.4578 (at 24° C.). The product was 95.7% pure.

后处理

本页导航参与物实验过程后处理来源与证据反应笔记
  • additionAfter the dropwise addition
  • additionThen the mixture was poured on to ice
  • extractionextracted
  • washThe organic phase was washed with sodium hydrogencarbonate solution
  • dry with materialdried over sodium sulphate
  • concentrationconcentrated
  • customa rotary evaporator
  • distillationThe crude product was distilled under an oil pump vacuum
  • customof 1.4578 (at 24° C.)
  • 来源与证据

    ORD记录
    ord-afec642ef1af4c7c96b1e22144e82fe1
    来源数据集
    uspto-grants-1992_06
    DOI
    10.6084/m9.figshare.5104873.v1
    专利号
    US05124476

    反应笔记

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