반응 #74961

반응 방정식

hexachlorocyclopentadiene

p-benzoquinone

→

1,2,3,4,9,9-hexachloro-1,4,4a,8a-tetrahydro-1,4-methanonaphthalene-5,8-dione

수율 64.0%

용매

toluene

toluene

반응 조건

후처리

1. 1
   workup.ADDITIONA mixture of 54.6 g
2. 2
   온도refluxed gently
3. 3
   기타completion of the reaction
4. 4
   세척rinsed with absolute ethanol
5. 5
   기타dried on the funnel
6. 6
   기타crystallized from ethanol
7. 7
   기타of bright yellow dense crystals were obtained
8. 8
   기타m.p. 189°-193° C. (reported 188° C.)

실험 절차

A mixture of 54.6 g. (0.2 mole) of hexachlorocyclopentadiene, 21.6 g. (0.2 mole) of p-benzoquinone, and 10 ml. of toluene were placed in a 125 ml. round bottom flask and heated for three hours so that the toluene refluxed gently. At the end of this period the reaction mixture suddenly solidified completely, indicating completion of the reaction. The crude product was bright yellow. The damp material was transferred to a Buchner funnel, rinsed with absolute ethanol, dried on the funnel, and crystallized from ethanol. 49 g. of bright yellow dense crystals were obtained, m.p. 189°-193° C. (reported 188° C.). The yield was 64%.

출처