تفاعل #165261

معادلة التفاعل

acetic acid

2-fluoro-4-(5-fluoro-pyridin-2-ylmethoxy)-benzaldehyde

nitromethane

ammonium acetate

→

title compound

المردود 94.5%

5-Fluoro-2-(3-fluoro-4-((E)-2-nitro-vinyl)-phenoxymethyl)-pyridine

المردود 94.5%

المذيبات

ethyl acetate

Water

ظروف التفاعل

المعالجة

1. 1
   استخلاصthe organic layer was extracted with ethyl acetate
2. 2
   غسيلThe organic layer was washed with water and saturated aqueous sodium chloride
3. 3
   تجفيفdried over anhydrous magnesium sulfate
4. 4
   ترشيحfiltered
5. 5
   تركيزThe filtrate was concentrated under a reduced pressure

الإجراء التجريبي

To an acetic acid (20.0 mL) solution of 2-fluoro-4-(5-fluoro-pyridin-2-ylmethoxy)-benzaldehyde (901 mg, 3.62 mmol) described in Manufacturing Example 96-1-1 were added nitromethane (1.10 g, 18.1 mmol) and ammonium acetate (558 mg, 7.24 mmol) under nitrogen atmosphere, which was stirred for 2 hours at 110° C. Water and ethyl acetate were added to the reaction mixture, and the organic layer was extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure to obtain the title compound (1.00 g) as a crude product.

المصدر