반응 #311587

반응 방정식

2,4-bis(trichloromethyl)benzo[1,3]dioxin-6-carboxylic acid

ammonium chloride

sodium azide

→

4-dichloromethylene-2-trichloromethybenzo[1,3]dioxin-6-carboxylic acid

용매

dimethylsulphoxide

반응 조건

후처리

1. 1
   온도was warmed on the steam bath for 16 hours
2. 2
   온도The reaction mixture was cooled
3. 3
   workup.ADDITIONpoured onto ice
4. 4
   여과The white product was filtered off
5. 5
   세척washed with water
6. 6
   기타dried
7. 7
   기타crystallised from aqueous ethanol

실험 절차

A mixture of 2,4-bis(trichloromethyl)benzo[1,3]dioxin-6-carboxylic acid (2.08 g.), ammonium chloride (0.33 g.) and sodium azide (0.36 g.) in anhydrous dimethylsulphoxide (10 ml.) was warmed on the steam bath for 16 hours. The reaction mixture was cooled, poured onto ice and kept for 16 hours. The white product was filtered off, washed with water and dried, and crystallised from aqueous ethanol to give 4-dichloromethylene-2-trichloromethybenzo[1,3]dioxin-6-carboxylic acid, m.p. 222°-223° C.

출처