تفاعل #45919

ord-803d65da74664f0e8ad0f65cc171b8de

المذيبات

ظروف التفاعل

درجة الحرارة
90°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter cooling to rt
  2. 2
    أخرىthe reaction was quenched by cold H2O (50 mL)
  3. 3
    استخلاصthe resulting mixture was extracted with EtOAc (3×100 mL)
  4. 4
    غسيلThe combined EtOAc extracts were washed with brine (3×50 mL)
  5. 5
    تجفيفdried (anhydrous Na2SO4)
  6. 6
    أخرىThe solvent was removed in vacuo

الإجراء التجريبي

To a stirred solution of 3-hydroxybenzaldehyde (20 mmol) in DMSO (50 mL) at rt, solid Cs2CO3 (60 mmol) was added. 1-(2-chloroethyl)pyrrolidine hydrochloride (30 mmol) was added to the reaction mixture and heated to 90° C. for 9 h. After cooling to rt, the reaction was quenched by cold H2O (50 mL), and the resulting mixture was extracted with EtOAc (3×100 mL). The combined EtOAc extracts were washed with brine (3×50 mL) and dried (anhydrous Na2SO4). The solvent was removed in vacuo to afford crude 3-(2-pyrrolidin-1-yl-ethoxy)benzaldehyde.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07737285B2uspto-grants-2010_06