تفاعل #355758

ord-5dca1ffcee9c4e1fac40ef9667593d59

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas refluxed for 24 hours
  2. 2
    درجة الحرارةAfter cooling
  3. 3
    ترشيحthe reaction mixture was filtered
  4. 4
    أخرىthe solvent was evaporated
  5. 5
    أخرىThe product was recrystallized from methanol
  6. 6
    أخرىwas 103-104° C

الإجراء التجريبي

A mixture of 10 g (0.05 mol) of phenothiazine (obtained from Fluka), 11.7 g (0.075 mol) of iodoethane (obtained from Aldrich), 4.2 g (0.075 mol) of potassium hydroxide and 0.25 g of tetra-n-butylammonium hydrogen sulfate (obtained from Aldrich) in 200 ml of dry toluene was refluxed for 24 hours. After cooling, the reaction mixture was filtered and the solvent was evaporated. The product was recrystallized from methanol. The yield of 10-ethylphenothiazine (C14H13NS, FW=227.33) was 90%. The melting point of the product was 103-104° C. The 1H-NMR spectrum (100 MHz) of the product in CDCl3 was characterized by the following chemical shifts (δ, ppm): 1.40 (t, J=7.0 Hz, 3H, CH3); 3.90 (q, J=7.0 Hz, 2H, CH2); 6.78-7.32 (m, 8H, Ar).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07445877B2uspto-grants-2008_11