Methane → 2-Furylglyoxylic acid

The 24.5 g. of crude 2-furoylcyanide was mixed with 160 ml. concentrated hydrochloric acid at 25° C. with intermittent stirring. The reaction was stored for 24 hours at 25° C. and diluted with 80 ml. of water. The reaction was stirred for 5 minutes and filtered. The filtrate was saturated with sodium chloride and extracted with 5 × 120 ml. of 1:1 ether-ethyl acetate solution. The extracts were combined, dried over anhydrous magnesium sulfate and evaporated at 30° C. (15 mm.) to give a brownish-orange solid. The solid was dissolved in methanol, treated with charcoal and evaporated under reduced pressure (15 mm.) to dryness to yield 17 g. of the acid.

1. customat 25° C.
2. additiondiluted with 80 ml
3. filtrationfiltered
4. extractionextracted with 5 × 120 ml
5. dry with materialdried over anhydrous magnesium sulfate
6. customevaporated at 30° C. (15 mm.)
7. customto give a brownish-orange solid
8. customevaporated under reduced pressure (15 mm.) to dryness
9. customto yield 17 g

ORD record

ord-b07a481c2b874598a273772225e601fe

Source dataset

uspto-grants-1978_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04104469