تفاعل #2139932

ord-7d2196d0a09441f3bd870125976e9caa

معادلة التفاعل

c1ccc2c(c1)Nc1ccccc1S2
phenothiazine
CCI
iodoethane
[K+].[OH-]
potassium hydroxide
CCN1c2ccccc2Sc2ccccc21
10-Ethylphenothiazine

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 crystallized 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 crystallized from methanol. The yield of 10-ethylphenothiazine was 10.2 g (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: US07326506B2uspto-grants-2008_02