Sodium Hydroxide → HCID 59846870, compound

A stirred solution of 0.40 gram (0.0018 mole) of ethyl 5-chloro-4-nitropyrrole-2-carboxylate and 10 mL (excess) of an aqueous solution of 10% sodium hydroxide in 25 mL of methanol was warmed to 80° C. where it was maintained during a 1.5-hour period. After this time the reaction mixture was cooled and the methanol was removed under reduced pressure. The concentrate was diluted with 50 mL of water and 50 mL of ethyl acetate, and acidified to a pH of about 2.0. The organic layer was separated, dried with sodium sulfate, filtered, and the filtrate was concentrated under reduced pressure to a residue. The yield of the subject compound was 0.34 gram. The NMR spectrum was consistent with the proposed structure.

1. temperaturewas maintained during a 1.5-hour period
2. temperatureAfter this time the reaction mixture was cooled
3. customthe methanol was removed under reduced pressure
4. additionThe concentrate was diluted with 50 mL of water and 50 mL of ethyl acetate
5. customThe organic layer was separated
6. dry with materialdried with sodium sulfate
7. filtrationfiltered
8. concentrationthe filtrate was concentrated under reduced pressure to a residue

ORD record

ord-8bbe77b43e364d569b60298acb3f30bb

Source dataset

uspto-grants-2011_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07943642B2