تفاعل #215955

ord-19fe6cc18fd94628b72c94279e7141f8

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةheated
  2. 2
    درجة الحرارةto reflux for 2 hours
  3. 3
    أخرىThe nitroethane is then evaporated off under reduced pressure
  4. 4
    workup.ADDITIONis added
  5. 5
    أخرىAfter separation of the two phases
  6. 6
    غسيلthe organic phase is washed with water
  7. 7
    تجفيفThe organic phase is then dried over MgSO4
  8. 8
    تركيزconcentrated under reduced pressure
  9. 9
    أخرى2.59 g (10.64×10-3 mol) of the expected nitroethylenic compound (yellow solid) are then obtained, equivalent to a 95% yield

الإجراء التجريبي

2.13 g (11.20×10-3 mol) of naphthaldehyde, 30 cm3 of nitroethane and 0.54 g (7×10-3 mol) of ammonium acetate are introduced into a round-bottomed flask. The mixture is stirred and heated to reflux for 2 hours. The nitroethane is then evaporated off under reduced pressure, the residue is taken up with CH2Cl2 and water is added to hydrolyze the acetate. After separation of the two phases, the organic phase is washed with water, the aqueous phases with CH2Cl2 (twice). The organic phase is then dried over MgSO4 and concentrated under reduced pressure. 2.59 g (10.64×10-3 mol) of the expected nitroethylenic compound (yellow solid) are then obtained, equivalent to a 95% yield.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05464872uspto-grants-1995_11