反应详情

The starting material is prepared as follows: -chloro-2,3,4,5 suspension of 6.0 g of 8-chloro--tetrahydro-1-benzazepine-2,5-dione-4-carboxylic acid methyl ester in 125 ml of dimethyl formamide is added portion-wise to that of 2.1 g of a 57% mineral oil suspension of sodium hydride in 300 ml of dimethylformamide while stirring under argon. After stirring for 3 hours at room temperature 4.6 g of n-butyl iodide are added dropwise and stirring is continued over night at said temperature. The pH of the mixture is adjusted to 2 with 3N hydrochloric acid and the whole evaporated. The residue is partitioned between water and chloroform, the organic solution separated and the aqueous solution extracted with chloroform. The combined extract is washed with water, dried, evaporated and the residue taken up in diethyl ether. The mixture is treated with charcoal, filtered hot and the filtrate concentrated, to yield the 8-chloro-1-n-butyl-2,3,4,5-tetrahydro-1-benzazepine-2,5-dione-4-carboxylic acid methyl ester, melting at 89°-90°.

1. customThe starting material is prepared
2. additionis added portion-wise to that
3. additionare added dropwise
4. stirringstirring
5. waitis continued over night
6. customThe residue is partitioned between water and chloroform
7. customthe organic solution separated
8. extractionthe aqueous solution extracted with chloroform
9. extractionThe combined extract
10. washis washed with water
11. customdried
12. customevaporated
13. additionThe mixture is treated with charcoal
14. filtrationfiltered hot
15. concentrationthe filtrate concentrated