تفاعل #4936

ord-db521c60394943f7aa9b07de7bbb410c

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe solution was heated
  2. 2
    أخرىThe morpholine was then removed by rotary evaporation (90° C., vacuum pump)
  3. 3
    غسيلwashed with dilute aqueous sodium hydroxide (2×30 ml)
  4. 4
    تركيزThe organic layer was concentrated by rotary evaporation (60° C., water aspirator)
  5. 5
    أخرىThe residue was recrystallized from ethanol giving 3.26 g (60%) of light yellow crystals, m.p. 152°-153° C.

الإجراء التجريبي

2-(2-Chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepine-5(4H)-thione, 4.5 g (0.018 mole) was dissolved in morpholine (30 ml). The solution was heated with stirring to 50°-60° C. for 6 hr. The morpholine was then removed by rotary evaporation (90° C., vacuum pump). The residue was taken up in chloroform (100 ml) and washed with dilute aqueous sodium hydroxide (2×30 ml). The organic layer was concentrated by rotary evaporation (60° C., water aspirator). The residue was recrystallized from ethanol giving 3.26 g (60%) of light yellow crystals, m.p. 152°-153° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04727152uspto-grants-1988_02