تفاعل #64973

ord-7de3f40395fc4e26abc7714ca6ef2c32

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGThe mixture is stirred at 80° C. overnight
  2. 2
    درجة الحرارةcooled
  3. 3
    أخرىthe aqueous phase is separated off
  4. 4
    استخلاصextracted with toluene
  5. 5
    تجفيفThe toluene solutions are dried over K2CO3
  6. 6
    تركيزconcentrated
  7. 7
    workup.DISTILLATIONthe residue is distilled

الإجراء التجريبي

89 g (0.5 mol) of ethyl N-(2,2-dimethoxyethyl)-carbamate are added dropwise to 17.5 g (0.58 mol) of NaH (80% strength in paraffin oil) in 500 ml of absolute toluene at 80° C. The mixture is then stirred for one hour and 80 g (0.59 mol) of 1-bromo-2-butene are subsequently added dropwise at 80° C. The mixture is stirred at 80° C. overnight and cooled, the salts are dissolved with water and the aqueous phase is separated off and extracted with toluene. The toluene solutions are dried over K2CO3 and concentrated and the residue is distilled.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05416096uspto-grants-1995_05