반응 #4901

반응 방정식

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

phosphorus pentasulfide

→

2-(2-Chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-oxazepine-5(4H)-thione

용매

chloroform

반응 조건

후처리

1. 1
   온도the mixture was heated
2. 2
   온도to reflux for 18 hr
3. 3
   여과The mixture was filtered
4. 4
   추출the filtrate was extracted with dilute sodium hydroxide
5. 5
   농축The chloroform layer was concentrated
6. 6
   workup.DISSOLUTIONthe residue was dissolved in 250 ml of boiling isopropyl alcohol
7. 7
   온도On cooling
8. 8
   기타28 g (44%) of yellow solid precipitated
9. 9
   기타A portion was recrystallized from isopropyl alcohol, m.p. 134°-136° C.

실험 절차

To a solution of 59 g (0.25 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepin-5(4H)one hydrochloride in 1500 ml of chloroform was added 41.5 g (0.19 mole) of phosphorus pentasulfide and the mixture was heated to reflux for 18 hr. The mixture was filtered and the filtrate was extracted with dilute sodium hydroxide. The chloroform layer was concentrated and the residue was dissolved in 250 ml of boiling isopropyl alcohol. On cooling, 28 g (44%) of yellow solid precipitated. A portion was recrystallized from isopropyl alcohol, m.p. 134°-136° C.

출처