Hydrochloric Acid → 4-[1-(3-Bromo-5-methoxymethyl-thiophen-2-yl)-1-hydroxyimino-methyl]-piperidine-1-carboxylic acid tert-butyl ester

Add hydroxylamine hydrochloride (2.29 g, 45.27 mmol, 2.00 equivalents) to a stirred solution of 4-[1-(3-bromo-5-methoxymethyl-thiophen-2-yl)-methanoyl]-piperidine-1-carboxylic acid tert-butyl ester (9.47 g, 22.64 mmol, 1.00 equivalents) in pyridine (42.40 mL). Stir the resulting solution at room temperature overnight and then at 70° C. for 4 hours. Cool the reaction mixture slightly, add hydrochloric acid (3N, 100 mL) and extract the resulting mixture with dichloromethane (100 mL). Wash the extract with water (100 mL), dry over magnesium sulfate, filter and evaporate to yield the desired product as a yellow oil (9.48 g).

1. waitat 70° C. for 4 hours
2. temperatureCool the reaction mixture slightly
3. extractionextract the resulting mixture with dichloromethane (100 mL)
4. washWash the
5. extractionextract with water (100 mL)
6. dry with materialdry over magnesium sulfate
7. filtrationfilter
8. customevaporate

ORDレコード

ord-461d684a673b40babd15a4ca5f40cabe

出典データセット

uspto-grants-2009_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07550469B2