Reaktion #55616

ord-caf24c795a934682aa045ca65210c2ab

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter workup, the solid product was purified by column and high-pressure liquid chromatography

Vorschrift

A mixture of 4.54 g N-chloroacetyl-2,6-dimethylaniline and 3 g 3-methyl-5-chloromethylisoxazole (prepared as in Example 8 above) in 100 ml dry dimethylformamide was treated with 1.33 g sodium hydride as in Example 3 above. After workup, the solid product was purified by column and high-pressure liquid chromatography to yield 2.0 g pure product, m.p. 78°-82° C. This product is shown as Compound 1 in Table I. C15H17ClN2O2 : calc., %C 61.54, %H 5.81, %N 9.57; found, %C, 63.37, %H 6.16, %N 9.65.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04221584uspto-grants-1980_09