تفاعل #685480

ord-c1434a2777f34e4b907c7cc8ef82cbd1

المذيبات

ظروف التفاعل

درجة الحرارة
35°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىfitted with a calcium chloride drying tube
  2. 2
    أخرىA precipitate formed
  3. 3
    أخرىwas isolated by filtration
  4. 4
    غسيلwashed with deionized water (500 mL)
  5. 5
    أخرىdried under vacuum at 50° C.

الإجراء التجريبي

A mixture of 1-[7-benzyloxy-2-(hydroxymethyl)-1H-imidazo[4,5-c]quinolin-1-yl]-2-methylpropan-2-ol (39.0 g, 0.133 mol), pyridine (390 mL), and acetic anhydride (195 mL) was heated at 35±5° C. for one hour in a reaction flask fitted with a calcium chloride drying tube. The reaction mixture was poured into a mixture of ice (2.5 kg) and deionized water and stirred for approximately 15 minutes. A precipitate formed and was isolated by filtration, washed with deionized water (500 mL), and dried under vacuum at 50° C. to provide 41.8 g of [7-benzyloxy-1-(2-hydroxy-2-methylpropyl)-1H-imidazo[4,5-c]quinolin-2-yl]methyl acetate.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07897597B2uspto-grants-2011_03