ChemicalBook CAS DataBase List METHYL OXALYL CHLORIDE

METHYL OXALYL CHLORIDE synthesis

7synthesis methods

Product Name:METHYL OXALYL CHLORIDE
CAS Number:5781-53-3
Molecular formula:C3H3ClO3
Molecular Weight:122.51

67-56-1 Synthesis

67-56-1
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79-37-8
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5781-53-3
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$8.00/10g

Yield:5781-53-3 93%

Reaction Conditions:

in diethyl ether at 0; for 2 h;

Steps:

1 Synthesis of monomethyl oxalyl chloride

Oxalyl chloride (79.64 g, 627.5 mmol, 1.05 eq) was dissolved in diethylether (40 mL) and carefully mixed at0°C with a solution of methanol (19.15 g, 597.6 mmol, 1.00 eq) in diethylether (50 mL). The reaction mixture was stirredat 0°C for 2h and the crude product purified by distillation (bp 116°C). Monomethyl oxalyl chloride was isolated in 93%yield (68.05 g, 555.5 mmol). 1H-NMR (300 MHz, MeCN-d3): δ / ppm = 3.93 (s, 3H, COOCH3). 13C-NMR (75 MHz, MeCNd3):δ/ ppm = 162.4 (COCI), 156.8 (COOCH3), 56.0 (COOCH3).

References:

EP2940010,2015,A1 Location in patent:Paragraph 0127; 0128