تفاعل #42132
ord-91e1be0e020040e7aa4ba5c2fabcadab
معادلة التفاعل
الكواشف
لا شيء
المذيبات
ظروف التفاعل
درجة الحرارة
-10°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىBefore removing the ice-bath
- 2أخرىthe reaction was quenched
- 3workup.ADDITIONby adding water (0.5 L)
- 4أخرىThe aqueous layer was separated
- 5غسيلthe organic layer was washed with water (0.5 L) and brine (0.5 L)
- 6تجفيفdried over MgSO4
- 7ترشيحfiltered
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.