反应详情

温度

62.5 °C

Carbohexyl 1-chloroethyl carbonate (36 g) is added to a suspension of trityl candesartan (100 g), potassium carbonate (24 g) and potassium iodide (12 g) in DMSO (500 ml) at temperature of 60-65° C. over 30 min. Reaction mass is maintained at 60-65° C. for 2 hrs, added toluene (300 ml) and water (300 ml). Reaction mass is mixed for 15 min., allowed to settle, the layers are separated at 60-65° C. and aqueous layer is extracted with toluene (200 ml). Water (200 ml) washings are given to the combined organic layer and toluene extractions twice at temperature of 60-65° C. Toluene is distilled off from water washed organic layer at temperature below 60° C. under vacuum, ethanol (100 ml) is added, mixed for about 30 min and distilled off solvents under vacuum at temperature below 60° C. under vacuum. Residue is cooled to 30-35° C., ethanol (300 ml) is added, mixed for 2 hrs at 25-30° C. and filtered the product. Wet cake is washed with ethanol (100 ml) and suck dried. Wet weight of Cilexetil trityl candesartan is 180 g

1. customReaction mass
2. customReaction mass
3. additionis mixed for 15 min.
4. customthe layers are separated at 60-65° C.
5. extractionaqueous layer is extracted with toluene (200 ml)
6. extractionWater (200 ml) washings are given to the combined organic layer and toluene extractions twice at temperature of 60-65° C
7. distillationToluene is distilled off from water washed organic layer at temperature below 60° C. under vacuum, ethanol (100 ml)
8. additionis added
9. additionmixed for about 30 min
10. distillationdistilled off solvents under vacuum at temperature below 60° C. under vacuum
11. temperatureResidue is cooled to 30-35° C.
12. additionethanol (300 ml) is added
13. additionmixed for 2 hrs at 25-30° C.
14. filtrationfiltered the product
15. washWet cake is washed with ethanol (100 ml)
16. customsuck dried