تفاعل #445396

ord-f3461c3a4b8c4205b99d01f4209d939c

المذيبات

ظروف التفاعل

درجة الحرارة
5°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحthe mixture was filtered
  2. 2
    تركيزThe filtrate was concentrated
  3. 3
    استخلاصthe suspension was extracted with chloroform
  4. 4
    workup.ADDITIONEthereal hydrochloric acid was added to the organic phase
  5. 5
    أخرىthe reaction product which had precipitated
  6. 6
    ترشيحwas filtered off

الإجراء التجريبي

9.5 g (0.03 mole) of p-tert.-butyl-2-methyl-3-(2,6-dimethyl-morpholin-4-yl)-propiophenone were heated under reflux with 3.6 g (0.05 mole) of hydroxylamine hydrochloride in 80 ml of ethanol for 20 hours. After cooling to 5° C., the mixture was filtered. The filtrate was concentrated, the residue was suspended in dilute sodium hydroxide solution and the suspension was extracted with chloroform. Ethereal hydrochloric acid was added to the organic phase and the reaction product which had precipitated was filtered off. 10.6 g (96% of theory) of p-tert.-butyl-2-methyl-3-(2,6-dimethyl-morpholin-4-yl)-propiophenone oxime hydrochloride of melting point 214° to 16° C. were obtained.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04465678uspto-grants-1984_08