Tetracycline compound with amino acid amidine
A compound, aminosulfonyl technology, applied in the field of medicine, can solve the problems of inconvenient medication, patient pain, less than ideal gram-negative bacteria activity, etc.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0098] Example 1 [S-(4α, 12aα)]-9-amino-4,7-bis(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3, 10,12,12a-Tetrahydroxy Preparation of 1,11-dioxo-2-naphthalenamide dihydrochloride
[0099] Throw 5.3g (0.01mol) [S-(4α,12aα)]-9-amino-4,7-bis(dimethylamino)-1,4,4a,5,5a,6,11 into the reaction bottle , 12a-octahydro-3,10,12,12a-tetrahydroxy-1,11-dioxo-2-naphthacenecarboxamide dihydrochloride, dissolved in 70mL of concentrated sulfuric acid, cooled in an ice bath under stirring , and then 1.3 g of sodium nitrate was added, and the mixture was stirred in an ice bath for 1 h. After the reaction was completed, the mixture was added dropwise into 800 mL of diethyl ether, and a solid precipitated out, which was washed with a small amount of diethyl ether and dried. Add the solid to 20 mL of ethanol, then add 0.4 g of 10% palladium carbon, and stir at room temperature for 1 h under a hydrogen pressure of 2 MPa. After filtration and concentration under reduced pressure, 200 mL of di...
Embodiment 2
[0100] Example 2 [S-(4α, 12aα)]-9-[2-(tert-butylamino)acetamidoyl]-4,7-bis(dimethylamino)-1,4,4a,5,5a,6 , 11, 12a-octahydro - Preparation of 3,10,12,12a-tetrahydroxyl-1,11-dioxo-2-naphthacenecarboxamide (compound 1)
[0101] Add 50mL of 10% HCl-ethanol, 8.5g (42mmol) of 2-(benzyl (tert-butyl)amino) acetonitrile into the reaction flask, stir at room temperature for 0.5h, distill off the solvent under reduced pressure, then add 100mL of ethanol to dissolve , and then slowly add [S-(4α,12aα)]-9-amino-4,7-bis(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro -3,10,12,12a-Tetrahydroxy-1,11-dioxo-2-naphthalene carboxamide dihydrochloride 18g (33mmol), reflux and stir for 5h, after the reaction is complete, add 0.4g 10 % palladium carbon, stirred at 45° C. for 2 h under 1 MPa hydrogen pressure. After filtration, the filtrate was concentrated under reduced pressure to 1 / 3 of the original volume, and was added dropwise to 100 mL of diethyl ether containing 6 mL of triethylamine under...
Embodiment 3
[0106] Example 3 [S-(4α, 12aα)]-9-[2-(N,N-dimethylamino)-acetamido]-4,7-bis(dimethylamino)-1,4, 4a, 5, 5a, 6, 11, 12a- Preparation of octahydro-3,10,12,12a-tetrahydroxy-1,11-dioxo-2-naphthacenecarboxamide (Compound 2)
[0107] Add 50mL of 10% HCl-ethanol and 3.4g (40mmol) of 2-(N,N-dimethylamino)acetonitrile into the reaction flask, stir at room temperature for 0.5h, distill off the solvent under reduced pressure, then add 100mL of ethanol to dissolve, Then slowly add [S-(4α,12aα)]-9-amino-4,7-bis(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro- 3,10,12,12a-Tetrahydroxy-1,11-dioxo-2-naphthacenecarboxamide dihydrochloride 18g (33mmol), reflux and stir for 5h, after reaction, concentrate the reaction solution under reduced pressure to the original volume 1 / 3 was added dropwise to 100 mL of diethyl ether containing 6 mL of triethylamine under ice-cooling, and a solid was precipitated, filtered and dried to obtain 13.4 g of the target compound, yield: 73.2%.
[0108] Molecular...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More 


