反应详情

To the water solution of 1-(3,4-dichlorophenyl)-2-methylisothiourea hydroiodide was added saturated Na2CO3 solution at ice cold temperature till the pH reached about 9 to about 10. The reaction mixture was extracted with CHCl3 three times. The chloroform extracts were combined and dried over Na2SO4. The solvent was removed in vacuo to give crude product (13) as a white solid in quantitative yield, mp 166° C. The product was pure enough for further reaction. 1H NMR (600 MHz, CDCl3) δ 7.34(d, J=8.4 Hz, 1H), 7.02 (d, J=2.4 Hz, 1H), 6.75 (dd, 8.4 and 2.4 Hz, 1H), 4.58 (s, 2H), 2.42 (s, 3H); 13C NMR: δ 157.14, 148.74, 133.24, 131.31, 126.80, 124.23, 122.09, 14.16.

1. extractionThe reaction mixture was extracted with CHCl3 three times
2. dry with materialdried over Na2SO4
3. customThe solvent was removed in vacuo