反应详情

温度

0 °C

5.8 ml (3.3 eq.) of DIEA is added dropwise to a solution of 2.43 g (10 mmoles) of 10H-phenothiazine-2-carboxylic acid, 1.79 g (2.2 eq.) of ethylamine hydrochloride and 4.17 g (1.1 eq.) of HBTU in 50 ml of DMF, cooled down to 0° C. The reaction mixture is stirred for 15 hours at 23° C., and then poured into a mixture of 100 ml of a saturated solution of NaHCO3 and 100 ml of AcOEt. After stirring for a few minutes, the precipitate formed is removed by filtration and the filtrate is decanted. The organic phase is successively washed with water, a 1M solution of citric acid and salt water. The organic solution is dried over sodium sulphate, filtered and concentrated to dryness under vacuum. The solid obtained is suspended in Et2O, triturated and filtered. A beige solid is obtained with a quantitative yield. Melting point: 150-151° C.

1. stirringAfter stirring for a few minutes
2. customthe precipitate formed
3. customis removed by filtration
4. customthe filtrate is decanted
5. washThe organic phase is successively washed with water
6. dry with materialThe organic solution is dried over sodium sulphate
7. filtrationfiltered
8. concentrationconcentrated to dryness under vacuum
9. customThe solid obtained
10. customtriturated
11. filtrationfiltered
12. customA beige solid is obtained with a quantitative yield