تفاعل #169847
ord-e7b8ca838475418c88e53e5d7ee8864d
معادلة التفاعل
water
4-(benzyloxy)aniline
DIEA
methyl 2-fluoro-4-(trifluoromethyl)pyridine-3-carboxylate
→
title compound
المردود 11.0%
methyl 2-{[4-(benzyloxy)phenyl]amino}-4-(trifluoromethyl)pyridine-3-carboxylate
المردود 11.0%
الكواشف
لا شيء
المذيبات
ظروف التفاعل
درجة الحرارة
200°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1استخلاصthe mixture was extracted with EtOAc
- 2أخرىThe organic layer was separated
- 3غسيلwashed with water and brine
- 4تجفيفdried over Na2SO4
- 5تركيزconcentrated in vacuo
- 6أخرىThe residue was purified by column chromatography (silica gel, EtOAc/hexane)
الإجراء التجريبي
A mixture of 4-(benzyloxy)aniline (1010 mg), DIEA (1.771 mL) and methyl 2-fluoro-4-(trifluoromethyl)pyridine-3-carboxylate (1130 mg) in NMP (10 mL) was stirred at 150° C. for 2 h and at 200° C. for 1 h under microwave irradiation. The mixture was poured into water, and the mixture was extracted with EtOAc. The organic layer was separated, washed with water and brine, dried over Na2SO4 and concentrated in vacuo. The residue was purified by column chromatography (silica gel, EtOAc/hexane) to give the title compound (225 mg).