反应详情

To a stirred suspension of 4-amino-5-chloro-N-[2-(diethylamino)ethyl]-2-hydroxybenzamide hydrochloride (1.94 g, 6 mmoles) and potassium carbonate (4.16 g, 30 mmoles) in DMF (10 ml) was added 3-chloro-2-butanone (0.95 g, 8.9 mmoles) and the mixture stirred for 3 hours, followed by pouring into water and extraction with methylene chloride. The extract was washed well with water, dried and concentrated in vacuo. The residue was dissolved in 1-propanol and treated with 2N HCl followed by concentration to give an oily residue. This was crystallized from acetone and the product recrystallized from 2-propanol to give 1.4 g of the title compound mp 98° C. as the hemihydrate.

1. washThe extract was washed well with water
2. customdried
3. concentrationconcentrated in vacuo
4. dissolutionThe residue was dissolved in 1-propanol
5. additiontreated with 2N HCl
6. concentrationfollowed by concentration
7. customto give an oily residue
8. customThis was crystallized from acetone
9. customthe product recrystallized from 2-propanol