반응 #730368

ord-2577b84cc177486b9b1012e05d9563ea

용매

반응 조건

온도
5°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated to a gradually elevated temperature
  2. 2
    workup.STIRRINGstirred at room temperature for 10 hours
  3. 3
    기타the reaction
  4. 4
    여과The reaction mixture was filtered
  5. 5
    기타the solids obtained
  6. 6
    세척were washed with 150 g of toluene and 150 g of acetone
  7. 7
    기타dried in a vacuum

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07700243B2uspto-grants-2010_04