تفاعل #42132

ord-91e1be0e020040e7aa4ba5c2fabcadab

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
-10°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىBefore removing the ice-bath
  2. 2
    أخرىthe reaction was quenched
  3. 3
    workup.ADDITIONby adding water (0.5 L)
  4. 4
    أخرىThe aqueous layer was separated
  5. 5
    غسيلthe organic layer was washed with water (0.5 L) and brine (0.5 L)
  6. 6
    تجفيفdried over MgSO4
  7. 7
    ترشيحfiltered

الإجراء التجريبي

To a 3-necked 2-L flask was added N-benzyl-N-methylethanolamine (30.5 g, 0.182 mol), DCM (0.5 L), DIPEA (95 mL, 0.546 mol) and DMSO (41 mL, 0.728 mol). Using an ice bath, the mixture was cooled to about −10° C. and sulfur trioxide pyridine-complex (87 g, 0.546 mol) was added in 4 portions over 5 minute intervals. The reaction was stirred at −10° C. for 2 hours. Before removing the ice-bath, the reaction was quenched by adding water (0.5 L). The aqueous layer was separated and the organic layer was washed with water (0.5 L) and brine (0.5 L) and then dried over MgSO4 and filtered to provide the title compound which was used without further purification.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07728144B2uspto-grants-2010_06