Carbon Tetrachloride → HCID 67171120、化合物
反応式
[CH3:1][O:2][C:3]([C:5]1[CH:15]=[C:14]([Si](CC)(CC)CC)[C:8]2[O:9][C:10]([F:13])([F:12])[O:11][C:7]=2[CH:6]=1)=[O:4].C(Cl)(Cl)(Cl)Cl.[I:28]Cl>C(Cl)Cl>[CH3:1][O:2][C:3]([C:5]1[CH:15]=[C:14]([I:28])[C:8]2[O:9][C:10]([F:13])([F:12])[O:11][C:7]=2[CH:6]=1)=[O:4]参加物
5
反応条件
- 温度
- 77 °C
実験手順
17.0 g of 2,2-difluoro-7-triethylsilanyl-benzo[1,3]dioxole-5-carboxylic acid methyl ester were dissolved using 100 ml of CCl4 and 2.9 ml of ICl added. The mixture was then stirred for 3 h at 77° C., 1.5 ml of ICl added and stirred for 2 h at 77° C. The mixture was then allowed to cool to room temperature, 200 ml of CH2Cl2 added, and washed three times using 300 ml of a saturated aqueous Na2SO3-solution each. The organic layer was then dried using MgSO4 and evaporated. Chromatography on silica gel using EA/HEP 1:20 yielded 10.2 g of the title compound, colorless oil. Rf (EA/HEP 1:20)=0.30