반응 #4912

반응 방정식

7-Chloro-2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido [3,2-f][1,4]oxazepin-5(4H)-one

2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide

→

7-Chloro-2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepin-5(4H)thione

용매

toluene

반응 조건

후처리

1. 1
   온도The mixture was heated
2. 2
   온도to reflux
3. 3
   workup.STIRRINGthe mixture stirred
4. 4
   온도at reflux for 2 hr
5. 5
   workup.WAITleft
6. 6
   workup.WAITstanding for 56 hr at room temperature
7. 7
   기타The toluene layer was decanted
8. 8
   세척washed with 50 ml of dilute aqueous sodium hydroxide and 50 ml of dilute hydrochloric acid
9. 9
   기타Toluene was removed by rotary evaporation (~80° C., water aspirator)
10. 10
    기타The crude oil was recrystallized from isopropyl alcohol giving 3.5 g (54%) of pale yellow crystals, m.p. 125°-127° C.

실험 절차

7-Chloro-2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido [3,2-f][1,4]oxazepin-5(4H)-one, 6.0 g (0.022 mole) was suspended in 200 ml of toluene. To this suspension was added 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-dilsulfide. The mixture was heated to reflux with vigorous stirring for 2 hours. Because the reaction was not complete, an additional amount (3.0 g) of 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide was added and the mixture stirred at reflux for 2 hr and left standing for 56 hr at room temperature. The toluene layer was decanted and washed with 50 ml of dilute aqueous sodium hydroxide and 50 ml of dilute hydrochloric acid. Toluene was removed by rotary evaporation (~80° C., water aspirator). The crude oil was recrystallized from isopropyl alcohol giving 3.5 g (54%) of pale yellow crystals, m.p. 125°-127° C.

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