Реакция #6674

Уравнение реакции

potassium hydroxide

Phosphorus oxychloride

dimethylformamide

10-ethylphenothiazine

DMF

→

10-Ethylphenothiazine-3-carbaldehyde

Условия реакции

Обработка

1. 1
   ТемператураThe reaction mixture was refluxed at 80° C. for 24 hours
2. 2
   ЭкстракцияThe product was extracted with chloroform
3. 3
   ЭкстракцияThe chloroform extract
4. 4
   Сушкаwas dried with anhydrous sodium sulfate
5. 5
   Фильтрацияfiltered
6. 6
   workup.DISTILLATIONdistilled
7. 7
   ДругоеThe product was crystallized from methanol

Методика

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%.

Источник