3,5-DICHLORO-6-METHYL-1,4-OXAZIN-2-ONE synthesis
- Product Name:3,5-DICHLORO-6-METHYL-1,4-OXAZIN-2-ONE
- CAS Number:125849-94-7
- Molecular formula:C5H3Cl2NO2
- Molecular Weight:179.99
78-97-7
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$66.09/25ml
125849-94-7
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$130.00/100mg
Yield:-
Reaction Conditions:
with oxalyl dichloride;triethylamine hydrochloride in chlorobenzene at 0 - 90;Inert atmosphere;
Steps:
1 Step 1: 3,5-Dichloro-6-methyl-2H-1,4-oxazin-2-one
Into a 10-L 4-necked round-bottom flask was charged oxalic dichloride (3.32 kg, 26.2 mol) and chlorobenzene (3.5 L) under an inert atmosphere of nitrogen. A solution of 2- hydroxypropanenitrile (464.8 g, 6.54 mol) in chlorobenzene (500 mL) was added dropwise to the flask at 0 °C. The system was heated to 90 °C and triethylamine hydrochloride (66.2 g, 481 mmol) was added in portions at 90 °C. The resulting solution was stirred for 3 h before concentrating the mixture under reduced pressure. The resulting solution was diluted with ether (5 L) and the solids were filtered out. The filtrate concentrated and was then applied purified by silica gel column chromatography (0:1-1:4 EtOAc:petroleum ether) to yield the title compound.
References:
MERCK SHARP & DOHME CORP.;GAO, Xiaolei;KNOWLES, Sandra, L.;LI, Chunsing;LO, Michael Man-Chu;MAZZOLA, Robert, D., Jr.;ONDEYKA, Debra, L. WO2018/118736, 2018, A1 Location in patent:Page/Page column 53; 54
79-37-8
463 suppliers
$17.67/10gm:
78-97-7
2 suppliers
$66.09/25ml
125849-94-7
27 suppliers
$130.00/100mg
