반응 #334472

반응 방정식

2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-oxazepino[6,7-b]-quinolin-5(4H)-one

phosphorus pentasulfide

→

yellow crystals

수율 86.9%

2-(2-Chloroethyl)-2,3-dihydro-4-methyl-1,4-oxazepino[6,7-b]quinoline-5(4H)-thione

수율 86.9%

용매

toluene

acetonitrile

반응 조건

후처리

1. 1
   온도at reflux for 2 hr
2. 2
   온도After cooling
3. 3
   여과filtered
4. 4
   세척The residue on the filter paper was washed with 50 ml of additional toluene/acetonitrile, 3/1, V/V
5. 5
   세척The filtrate was washed with 3×50 ml saturated sodium carbonate (caution: gas evolved)
6. 6
   건조dried over anhydrous sodium sulfate
7. 7
   여과filtered
8. 8
   workup.ADDITIONtreated with activated charcoal
9. 9
   여과filtered again
10. 10
    농축concentrated by rotary evaporation (90° C., 30 mm)
11. 11
    기타The residual syrup was crystallized from isopropyl alcohol

실험 절차

To 3.0 g (0.01 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-oxazepino[6,7-b]-quinolin-5(4H)-one in 30 ml of acetonitrile was added 1.3 g (0.006 mole) of phosphorus pentasulfide. The mixture was stirred vigorously at reflux for 2 hr. After cooling, the reaction mixture was diluted with 60 ml of toluene and filtered. The residue on the filter paper was washed with 50 ml of additional toluene/acetonitrile, 3/1, V/V. The filtrate was washed with 3×50 ml saturated sodium carbonate (caution: gas evolved), dried over anhydrous sodium sulfate, filtered, treated with activated charcoal, filtered again and concentrated by rotary evaporation (90° C., 30 mm). The residual syrup was crystallized from isopropyl alcohol, yielding 1.6 g (52%) of yellow crystals, m.p. 114°-116° C.

출처