반응 #2139932

반응 방정식

phenothiazine

iodoethane

potassium hydroxide

→

10-Ethylphenothiazine

용매

toluene

반응 조건

후처리

1. 1
   온도was refluxed for 24 hours
2. 2
   온도After cooling
3. 3
   여과the reaction mixture was filtered
4. 4
   기타the solvent was evaporated
5. 5
   기타The product was crystallized from methanol
6. 6
   기타was 103-104° C

실험 절차

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).

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