تفاعل #40770

ord-d84e1cfa1e914306a388d7fad0ad38b1

معادلة التفاعل

CC(=O)c1ccc(Cl)cc1
p-chloroacetophenone
CNC.Cl
dimethylamine hydrochloride
C=O
paraformaldehyde
Cl
HCl
CN(C)CCC(=O)c1ccc(Cl)cc1.Cl
product
المردود 112.0%
CN(C)CCC(=O)c1ccc(Cl)cc1.Cl
1-(4-Chloro-phenyl)-3-dimethylamino-propan-1-one hydrochloride
المردود 112.0%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
40°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe mixture was refluxed for 5 h
  2. 2
    درجة الحرارةwas cooled further to 20° C
  3. 3
    ترشيحThe precipitate was filtered
  4. 4
    غسيلwashed with acetone and PA, and air
  5. 5
    أخرىdried

الإجراء التجريبي

To EtOH (80 mL), p-chloroacetophenone (77.3 g, 0.50 mol), dimethylamine hydrochloride (52.7 g, 0.65 mol), paraformaldehyde (19.8 g, 0.66 mol) and concentrated aqueous HCl (1 mL) were added and the mixture was refluxed for 5 h. The mixture was cooled to 40° C., acetone (400 mL) was added, and under stirring the mixture was cooled further to 20° C. The precipitate was filtered, washed with acetone and PA, and air dried to obtain 69.5 g of product which was used without further purification in the subsequent step.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07728018B2uspto-grants-2010_06