反応 #6674

反応方程式

potassium hydroxide

Phosphorus oxychloride

dimethylformamide

10-ethylphenothiazine

DMF

→

10-Ethylphenothiazine-3-carbaldehyde

反応条件

後処理

1. 1
   温度The reaction mixture was refluxed at 80° C. for 24 hours
2. 2
   抽出The product was extracted with chloroform
3. 3
   抽出The chloroform extract
4. 4
   乾燥was dried with anhydrous sodium sulfate
5. 5
   ろ過filtered
6. 6
   workup.DISTILLATIONdistilled
7. 7
   その他The product was crystallized from methanol

実験手順

Phosphorus oxychloride (POCl3,3.7 ml, 0.04 mol) was added dropwise to 4.4 ml (0.06 mol) of dry dimethylformamide (DMF) at 0° C. under a nitrogen atmosphere. This solution was warmed up slowly to room temperature. Then, a solution of 5 g (0.02 mol) of 10-ethylphenothiazine in dry DMF was added dropwise. The reaction mixture was refluxed at 80° C. for 24 hours and poured into the ice water. This solution was neutralized with potassium hydroxide until the pH reached 6–8. The product was extracted with chloroform. The chloroform extract was dried with anhydrous sodium sulfate, filtered and distilled. The product was crystallized from methanol. The yield of 10-ethylphenothiazine-3-carbaldehyde (C15H13NOS, FW=255.34) was 65%.

出典