反应详情

To a suspension of 17.4 g (0.043 mole) of 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diposphetane-2,4-disulfide in ~300 ml of toluene was added 20 g (0.078 mole) of 2-(2-chloroethyl)-2,3-dihydro-4,8-dimethylpyrido[3,2-f][1,4]-oxazepin-5(4H)-one hydrate [1:1]. The mixture was heated to reflux for 3 hr and 4.0 g (0.01 mole) of 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide was added and heating was continued for 1 hr. After cooling, toluene was decanted off and washed with 3×100 ml 1N sodium hydroxide and 100 ml water. The organic layer was then extracted with 2×100 ml of 2N hydrochloric acid. The aqueous layer was made just basic to litmus with conc. sodium hydroxide causing the product to precipitate out. Of the 25 g of crude collected, 2 g were recrystallized from diisopropyl ether to give pale yellow crystals, m.p. 80°-86° C.

1. temperatureThe mixture was heated
2. temperatureto reflux for 3 hr
3. temperatureheating
4. temperatureAfter cooling
5. customtoluene was decanted off
6. washwashed with 3×100 ml 1N sodium hydroxide and 100 ml water
7. extractionThe organic layer was then extracted with 2×100 ml of 2N hydrochloric acid
8. customto precipitate out
9. customOf the 25 g of crude collected
10. custom2 g were recrystallized from diisopropyl ether
11. customto give pale yellow crystals, m.p. 80°-86° C.