تفاعل #730368

ord-2577b84cc177486b9b1012e05d9563ea

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
5°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةheated to a gradually elevated temperature
  2. 2
    workup.STIRRINGstirred at room temperature for 10 hours
  3. 3
    أخرىthe reaction
  4. 4
    ترشيحThe reaction mixture was filtered
  5. 5
    أخرىthe solids obtained
  6. 6
    غسيلwere washed with 150 g of toluene and 150 g of acetone
  7. 7
    أخرىdried in a vacuum

الإجراء التجريبي

A 30.0 g quantity of N,N diethyl-N-methvlamine (reagent, product of Tokyo Kasei Co., Ltd.) was dissolved in 120 g of toluene, followed by nitrogen replacement. Over a period of 1 hour, 31.2 g of chloromethyl methyl ether (reagent, product of Tokyo Kasei Co., Ltd.) was added dropwise to the solution at 5° C. The mixture was stirred at 5° C. for 1 hour, heated to a gradually elevated temperature and stirred at room temperature for 10 hours to complete the reaction. The reaction mixture was filtered, and the solids obtained were washed with 150 g of toluene and 150 g of acetone and then dried in a vacuum, giving 53.7 g of the desired product (white solid).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07700243B2uspto-grants-2010_04