Реакция #474157

Уравнение реакции

1,2-cyclohexanedione

morpholine

N2

→

title compound

Выход 95.4%

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

Выход 95.4%

Растворители

toluene

Условия реакции

Обработка

1. 1
   ДругоеSynthesis
2. 2
   ДругоеA 500-mL round-bottomed flask is equipped with a Dean Stark, condenser
3. 3
   ТемператураThe resulting yellow solution is heated
4. 4
   Температураto reflux for 5 hours
5. 5
   ТемператураHeating
6. 6
   Другоеabout 3.0 mL of water are collected on the Dean Stark
7. 7
   ДругоеThe brown solution is decanted away from a thick oil
8. 8
   Промывкаrinsed with toluene
9. 9
   КонцентрированиеThe solution is concentrated under high vacuum
10. 10
    Другоеto afford

Методика

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.

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