반응 #474157

반응 방정식

1,2-cyclohexanedione

morpholine

N2

→

title compound

수율 95.4%

2-(morpholin-4-yl)-2-cyclohexen-1-one

수율 95.4%

용매

toluene

반응 조건

후처리

1. 1
   기타Synthesis
2. 2
   기타A 500-mL round-bottomed flask is equipped with a Dean Stark, condenser
3. 3
   온도The resulting yellow solution is heated
4. 4
   온도to reflux for 5 hours
5. 5
   온도Heating
6. 6
   기타about 3.0 mL of water are collected on the Dean Stark
7. 7
   기타The brown solution is decanted away from a thick oil
8. 8
   세척rinsed with toluene
9. 9
   농축The solution is concentrated under high vacuum
10. 10
    기타to afford

실험 절차

Synthesis based on literature modified procedure (Ōhashi, M.; Takahashi, T.; Inoue, S.; Sato, K. Bulletin Chemical Society of Japan, 1975; 48:1892). A 500-mL round-bottomed flask is equipped with a Dean Stark, condenser, stir bar and gas inlet (N2 gas atmosphere). The flask is charged with of 1,2-cyclohexanedione (15.14 g, 135.00 mmol), morpholine (14.82 g, 170.10 mmol) and toluene (330 mL). The resulting yellow solution is heated to reflux for 5 hours. Heating is stopped and about 3.0 mL of water are collected on the Dean Stark. The brown solution is decanted away from a thick oil and rinsed with toluene. The solution is concentrated under high vacuum to afford 23.33 g (95.34% yield) of title compound of Preparation 2 as a brown solid.

출처