تفاعل #334002

ord-d895fa1219154dfe9978b798b255f813

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe methylene chloride removed via evaporation
  2. 2
    أخرىis hydrogenated at atmospheric pressure and room temperature in the presence of methanesulphonic acid (2.4 g) and 10% palladium on charcoal (0.4 g)
  3. 3
    أخرىAfter the calculated quantity of hydrogen is consumed (510 ml)
  4. 4
    ترشيحthe solution is filtered
  5. 5
    أخرىthe ethanol is removed via evaporation
  6. 6
    استخلاصthe resulting solution is extracted with ether
  7. 7
    أخرىEvaporation of the dried ether
  8. 8
    استخلاصextract

الإجراء التجريبي

A mixture of (2,3-dihydro-1,4-benzodioxin-2-yl)methylamine (4.13 g), benzaldehyde (2.65 g) and methylene chloride (25 ml) is stirred for 3 hours at room temperature and the methylene chloride removed via evaporation. A solution of the residue in ethanol (30 ml) is hydrogenated at atmospheric pressure and room temperature in the presence of methanesulphonic acid (2.4 g) and 10% palladium on charcoal (0.4 g). After the calculated quantity of hydrogen is consumed (510 ml), the solution is filtered, the ethanol is removed via evaporation, the residue is made alkaline with saturated aqueous potassium carbonate, and the resulting solution is extracted with ether. Evaporation of the dried ether extract yields an oily residue of N-benzyl-(2,3-dihydro-1,4-benzodioxin-2-yl)methylamine (5.9 g).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04704389uspto-grants-1987_11