تفاعل #334533

معادلة التفاعل

dimethyl sulfoxide

2-(2-chloroethyl)-2,3-dihydro-4-methyl-7-(trifluoromethyl)-1,4-benzoxazepin-5(4H)-one

azetidine

potassium carbonate

azetidine

→

2-[2-(1-Azetidinyl)ethyl]-2,3-dihydro-4-methyl-7-(trifluoromethyl)-1,4-benzoxazepin-5(4H)-one oxalate

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   workup.WAITAfter 48 hr
2. 2
   استخلاصextracted with 3×100 ml of toluene
3. 3
   غسيلThe combined organic extracts were washed with 2×150 ml of water
4. 4
   تجفيفdried over anhydrous sodium sulfate
5. 5
   ترشيحfiltered
6. 6
   تركيزconcentrated by rotary evaporation
7. 7
   workup.ADDITIONThe residue was treated with oxalic acid in isopropyl alcohol
8. 8
   أخرىto give 3.0 g (65%) of white analytically pure crystals, m.p. 163°-166° C.

الإجراء التجريبي

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.

المصدر