تفاعل #1383377

ord-6abc1cb076a7426eaa6a68c2012b415d

المذيبات

ظروف التفاعل

درجة الحرارة
105°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىequipped with a mechanical stirrer
  2. 2
    درجة الحرارةis maintained at this temperature for 150 minutes
  3. 3
    أخرىto yield a solution
  4. 4
    درجة الحرارةAfter cooling to 50° C.
  5. 5
    درجة الحرارةthe obtained suspension is maintained for 4 hours at room temperature
  6. 6
    ترشيحThe solid that separates is filtered
  7. 7
    غسيلwashed with methanol (0.3 L)
  8. 8
    أخرىdried in the oven at 45° C. for 4 hours
  9. 9
    أخرىyielding the compound of the title (56.3 g, 0.172 mol, yield: 90%)

الإجراء التجريبي

5-Amino-1,3-benzenedicarboxylic acid dimethyl ester (40.0 g, 191 mmol) and 2-amino-1,3-dihydroxypropane (104.5 g, 1.147 mol) are loaded into a 1 L vessel equipped with a mechanical stirrer, a thermometer and a refluxing refrigerator. The suspension is heated up to 105° C., and is maintained at this temperature for 150 minutes to yield a solution. After cooling to 50° C., methanol (0.7 L) is added and the obtained suspension is maintained for 4 hours at room temperature. The solid that separates is filtered, washed with methanol (0.3 L), and dried in the oven at 45° C. for 4 hours yielding the compound of the title (56.3 g, 0.172 mol, yield: 90%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07244864B2uspto-grants-2007_07