تفاعل #52132

ord-b5668c9cfbea4a36a23507b041ea0948

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرى3 hours
  2. 2
    أخرىat room temperature
  3. 3
    استخلاصextracted 3 times with 500 ml of methylene chloride
  4. 4
    تجفيفdried over magnesium sulfate
  5. 5
    أخرىevaporated under vacuum
  6. 6
    أخرىThe remaining oil is flash-chromatographed on silica gel (mobile phase: methylene chloride/hexane/acetone: 20/10/3)

الإجراء التجريبي

At 0° C., 100 g (506.9 millimoles) of dibenzyl-amine (dissolved in 300 ml of methylene chloride) is added dropwise to a thoroughly stirred suspension of 234.51 g (2.53 mol) of epichlorohydrin and 200 ml of 32% sodium hydroxide solution. The mixture is stirred for 2 hours at 0° C. and then 3 hours at room temperature. The mixture is diluted with 3 l of water and extracted 3 times with 500 ml of methylene chloride. The organic phases are combined, dried over magnesium sulfate, and evaporated under vacuum. The remaining oil is flash-chromatographed on silica gel (mobile phase: methylene chloride/hexane/acetone: 20/10/3).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06855309B2uspto-grants-2005_02