تفاعل #52567

ord-60a582a1f67047778e5b4ab65a829ff1

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
70°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىA 5-necked flask equipped with mechanical overhead stirrer, gas inlet tube
  2. 2
    درجة الحرارةreflux condenser
  3. 3
    أخرىGaseous HCl was bubbled through the mixture for 4 hours
  4. 4
    أخرىDuring this time a thick white precipitate formed
  5. 5
    درجة الحرارةThe suspension was cooled to 0° C.
  6. 6
    أخرىthe precipitate was isolated by vacuum filtration
  7. 7
    أخرىthe yellow powder was dried over night under vacuum

الإجراء التجريبي

A 5-necked flask equipped with mechanical overhead stirrer, gas inlet tube, reflux condenser and a thermometer was charged with 4-nitrophenol (100 g, 0.72 mol). Concentrated HCl 932%, 1.3 L), conc. H2SO4 (98%, 10 mL) and formaldehyde dimethylacetal (152.4 g, 2 moles) were added and the mixture was heated to 70° C. Gaseous HCl was bubbled through the mixture for 4 hours. During this time a thick white precipitate formed. The suspension was cooled to 0° C., the precipitate was isolated by vacuum filtration and the yellow powder was dried over night under vacuum to give 108.76 g of slightly impure 2-chloromethyl-4-nitrophenol (about 76% yield).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06855833B2uspto-grants-2005_02