METHYL OXALYL CHLORIDE synthesis
- Product Name:METHYL OXALYL CHLORIDE
- CAS Number:5781-53-3
- Molecular formula:C3H3ClO3
- Molecular Weight:122.51
67-56-1
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79-37-8
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5781-53-3
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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
10304-09-3
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