Sodium Hydroxide → HCID 12897089、化合物

Methyl 5-chloropyrrole-3-carboxylate (900 g.) was refluxed for 9 hours with 20 ml. of methanol and 10 ml. of 1 N sodium hydroxide. Methanol was removed by evaporation, the aqueous residue was diluted with approximately 10 ml. of water and extracted twice with ether. The aqueous phase was acidified with conc. hydrochloric acid and product extracted into ethyl acetate. The three ethyl acetate extracts were combined, washed with saturated sodium chloride, dried over anhydrous sodium sulfate and evaported to product (715 mg., m.p. 175°-178° C.). Recrystallization from methylene chloride/hexane afforded purified 5-chloropyrrole-3-carboxylic acid (300 mg., m.p. 178°-180° C.).

1. customMethanol was removed by evaporation
2. additionthe aqueous residue was diluted with approximately 10 ml
3. extractionof water and extracted twice with ether
4. extractionextracted into ethyl acetate
5. washwashed with saturated sodium chloride
6. dry with materialdried over anhydrous sodium sulfate
7. customRecrystallization from methylene chloride/hexane
8. customafforded
9. custompurified 5-chloropyrrole-3-carboxylic acid (300 mg., m.p. 178°-180° C.)

ORDレコード

ord-0d5950d80ec64e7a9af10fac8540442c

出典データセット

uspto-grants-1981_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04282242