Formaldehyde → 4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]-2-methyl-N-(hydroxymethyl) benzoic acid amide

In a solution of 7.00 g of 4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]-2-methyl benzoic acid amide synthesized in Step 1 of Synthetic Example 19 in 70 mL of 1,4-dioxane, 1.82 g of 37% formalin, 7.00 g of potasiium carbonate and 15 mL of water were added at room temperature with stirring, and stirred at the same temperature for 3 hours. After the completion of the reaction, the reaction mixture was diluted by adding 200 mL of ethyl acetate, washed with water (50 mL×1), and then dehydrated with and dried over saturated sodium chloride aqueous solution and then anhydrous magnesium sulfate, filtered through silica gel, and the solvent was distilled off under reduced pressure to obtain 7.00 g of the crude product as white crystal.

1. stirringstirred at the same temperature for 3 hours
2. customAfter the completion of the reaction
3. additionthe reaction mixture was diluted
4. washwashed with water (50 mL×1)
5. dry with materialdried over saturated sodium chloride aqueous solution
6. filtrationanhydrous magnesium sulfate, filtered through silica gel
7. distillationthe solvent was distilled off under reduced pressure

ORD 기록

ord-808fe4c3ee0442ae8ba53d913c39619c

출처 데이터셋

uspto-grants-2011_05

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07951828B1