反应详情

To 30 ml of dimethyl sulfoxide was added 3.5 g (0.011 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methyl-7-(trifluoromethyl)-1,4-benzoxazepin-5(4H)-one, 1.3 g (0.022 mole) of azetidine, and 10 g of potassium carbonate. The reaction mixture was stirred at room temperature for 24 hr and 1.18 g (0.021 mole) of azetidine was added. After 48 hr, the reaction mixture was poured into 500 ml of water and extracted with 3×100 ml of toluene. The combined organic extracts were washed with 2×150 ml of water, dried over anhydrous sodium sulfate, filtered, and concentrated by rotary evaporation. The residue was treated with oxalic acid in isopropyl alcohol to give 3.0 g (65%) of white analytically pure crystals, m.p. 163°-166° C.

1. waitAfter 48 hr
2. extractionextracted with 3×100 ml of toluene
3. washThe combined organic extracts were washed with 2×150 ml of water
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated by rotary evaporation
7. additionThe residue was treated with oxalic acid in isopropyl alcohol
8. customto give 3.0 g (65%) of white analytically pure crystals, m.p. 163°-166° C.