反应详情

To a solution of 8.64 g. of 4,9-dihydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-one in 100 ml. of dimethylformamide is added 2.1 g. of 50% sodium hydride in mineral oil. The mixture is stirred for one hour and 10.0 g. of 4-chloro-3-trifluoromethyl benzyl chloride and 10 mg of potassium iodide are added. The mixture is stirred for a prolonged period and the solvent is removed in vacuo. The residual gum is dissolved in methylene chloride, dried over magnesium sulfate and filtered through magnesol. The filtrate is evaporated to give tan crystals which are recrystallized from ethanol giving the desired product as off-white crystals, mp. 181°-183° C.

1. stirringThe mixture is stirred for a prolonged period
2. customthe solvent is removed in vacuo
3. dissolutionThe residual gum is dissolved in methylene chloride
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered through magnesol
6. customThe filtrate is evaporated
7. customto give tan crystals which
8. customare recrystallized from ethanol giving the desired product as off-white crystals, mp. 181°-183° C.