ChemicalBook CAS DataBase List 4-(4-NITROPHENYL)MORPHOLIN-3-ONE

4-(4-NITROPHENYL)MORPHOLIN-3-ONE synthesis

12synthesis methods

Product Name:4-(4-NITROPHENYL)MORPHOLIN-3-ONE
CAS Number:446292-04-2
Molecular formula:C10H10N2O4
Molecular Weight:222.2

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Yield:446292-04-2 97.7%

Reaction Conditions:

with sodium chlorite;sodium dihydrogenphosphate dihydrate in water;acetonitrile at 40; for 6 h;

Steps:

2 Example 2 Synthesis of compound of formula II

Add 16.9g 80% sodium chlorite (0.15mol) into 65mL water and stir to dissolve,Prepare an aqueous solution of sodium chlorite for use.
10.4g (0.05mol) of the compound of formula III prepared in Example 1,23.4g (0.15mol) sodium dihydrogen phosphate dihydrate,Add 300mL acetonitrile to the reaction flask and heat to 40°C,Drop the prepared sodium chlorite aqueous solution,After dripping in about 10 minutes, react at 40°C for 6 hours after dripping.After the reaction is monitored by HPLC,Let stand and separate, collect the organic phase, add 70mL ethyl acetate to extract the lower aqueous phase twice,Combine the organic phases and place in a cold water bath,Add about 100mL saturated sodium sulfite aqueous solution,Stir for 10 minutes, add 50mL ethyl acetate to the water phase and extract twice.Combine the organic phases again, add anhydrous sodium sulfate to dry,Concentrate under reduced pressure to obtain a pale yellow solid,Add 240 mL of mixed organic solution (petroleum ether: ethyl acetate = 5:1) and stir well for 20 minutes,After treatment, 10.8 g of a light yellow powder solid was obtained, with a yield of 97.7% and an HPLC purity of 98.3%.

References:

CN112939893,2021,A Location in patent:Paragraph 0042; 0049-0052

29518-11-4 Synthesis