反应详情

温度

0 °C

Lithium aluminum hydride (0.20 g, 5.27 mmole) is added to 15 ml dry diethylether. To this slurry is added 4-(3,4,5-trimethoxyphenyl)-1,3-dithiolane-2-thione (32) (1.0 g, 3.31 mmole) predissolved in 20 ml dry THF. The reaction is refluxed under an N2 atmosphere for 12 hours. The reaction is cooled to 0° C. and the excess hydride destroyed with H2O. The reaction mixture is acidified with 10% HCl and immediately extracted with diethyl ether. The organic layer is washed with H2O, dried over MgSO4, filtered and evaporated to a white solid (9.836 g, 97%). NMR: (DCDl3) 2.34,d,1H;2.95,m,1H;3.09,m,1H; 3.84,s,3H;3.87,s,6H;4.03,m,1H;6.53,s,2H. M.S. (IBu) 261 (100%). Melting Point: 72.5°-73.5° C. C,H,S Analysis: (theoretical, actual) C (50.74,50.85); H (6.19,6.20); S (24.63,24.53).

1. temperatureThe reaction is refluxed under an N2 atmosphere for 12 hours
2. customthe excess hydride destroyed with H2O
3. extractionimmediately extracted with diethyl ether
4. washThe organic layer is washed with H2O
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customevaporated to a white solid (9.836 g, 97%)