تفاعل #1664118

ord-d59bfad340734446a14733926ddaaf97

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwere charged into a glass reaction vessel
  2. 2
    أخرىequipped with a mechanical stirrer
  3. 3
    workup.ADDITIONthermometer and addition funnel
  4. 4
    درجة الحرارةThe mixture was cooled in an ice bath
  5. 5
    workup.ADDITIONAfter addition
  6. 6
    workup.STIRRINGwas completed stirring
  7. 7
    ترشيحAfter this time the mixture was filtered
  8. 8
    غسيلthe filtrate washed with dilute aqueous hydrochloric acid
  9. 9
    تجفيفThe washed filtrate was dried over anhydrous magnesium sulphate

الإجراء التجريبي

The dimethyl acetal of 2-(2,6-diethylanilino)acetaldehyde (13 grams), benzene (75 ml) and sodium carbonate (5.8 grams) dissolved in water (50 ml) were charged into a glass reaction vessel equipped with a mechanical stirrer, thermometer and addition funnel. The mixture was cooled in an ice bath and chloroacetyl chloride (6.2 grams) was added dropwise with stirring. After addition was completed stirring was continued and the reaction mixture was allowed to warm up to room temperature. After this time the mixture was filtered and the filtrate washed with dilute aqueous hydrochloric acid. The washed filtrate was dried over anhydrous magnesium sulphate and was stripped of solvent under reduced pressure to yield the desired product the dimethyl acetal of 2-[N-(α-chloroacetyl)-2,6-diethylanilino]acetaldehyde.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US03983174uspto-grants-1976_09