Tetracycline compound with amino isonitroso
A compound and carbamoyl technology, applied in the field of tetracycline compounds with aminooxime group, can solve the problems of inconvenient medication, pain for patients, unsatisfactory activity of gram-negative bacteria and the like
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Embodiment 1
[0123] Example 1 [S-(4α, 12aα)]-9-[2-(tert-butylamino)-1-hydroxyimino-ethylamino]-4,7-bis(dimethylamino)- 1, 4, 4a, 5, 5a, 6, 11, 12a-eight Preparation of Hydrogen-3,10,12,12a-Tetrahydroxy-1,11-dioxo-2-naphthacenecarboxamide (Compound 1)
[0124] Step 1 [S-(4α,12aα)]-9-amino-4,7-bis(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,10 , Preparation of 12,12a-tetrahydroxyl-1,11-dioxo-2-naphthacenecarboxamide dihydrochloride
[0125] 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 to 800 ml of ether, and a solid was precipitated, which was washed with a small amount of ether and...
Embodiment 2
[0134] Example 2 [S-(4α, 12aα)]-9-[2-(N, N-dimethylamino)-1-hydroxyimino-ethylamino]-4,7-bis(dimethylamine base)-1,4,4a,5,5a,6,11,12a-octahydro-3,10,12,12a-tetrahydroxy-1,11-dioxo-2-tetracenecarboxamide (compound 2) Preparation
[0135] Steps 1 and 2 are the same as in Example 1.
[0136] 3. Preparation method Referring to step 3 in Example 1, inject [S-(4α, 12aα)]-9-[(2-chloroacetyl)amino]-4,7-bis(dimethylamino)-1 , 4,4a,5,5a,6,11,12a-octahydro-3,10,12,12a-tetrahydroxy-1,11-dioxo-2-naphthacenecarboxamide 2.7g (5mmol), 0.7 g (15 mmol) dimethylamine. [S-(4α, 12aα)]-9-[2-(N,N-dimethylamino)-acetamido]-4,7-bis(dimethylamino)-1,4,4a, 2.2 g of 5, 5a, 6, 11, 12a-octahydro-3, 10, 12, 12a-tetrahydroxy-1, 11-dioxo-2-tetracenecarboxamide, yield: 78.5%.
[0137] 4. Preparation method Referring to step 4 in Example 1, cast [S-(4α, 12aα)]-9-[2-(N,N-dimethylamino)-acetamido]-4,7-bis( Dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,10,12,12a-tetrahydroxy-1,11-dioxo-2-tetracene Amid...
Embodiment 3
[0141] Example 3 [S-(4α, 12aα)]-9-[2-(N, N-diethylamino)-1-hydroxyimino-ethylamino]-4,7-bis(dimethylamine base)-1,4,4a,5,5a,6,11,12a-octahydro-3,10,12,12a-tetrahydroxy-1,11-dioxo-2-tetracenecarboxamide (compound 3) Preparation
[0142] Steps 1 and 2 are the same as in Example 1.
[0143] 3. Preparation method Referring to step 3 in Example 1, inject [S-(4α, 12aα)]-9-[(2-chloroacetyl)amino]-4,7-bis(dimethylamino)-1 , 4,4a,5,5a,6,11,12a-octahydro-3,10,12,12a-tetrahydroxy-1,11-dioxo-2-naphthacenecarboxamide 2.7g (5mmol), 1.1 g (15 mmol) diethylamine. [S-(4α, 12aα)]-9-[2-(N,N-diethylamino)-acetamido]-4,7-bis(dimethylamino)-1,4,4a, Preparation of 5,5a,6,11,12a-octahydro-3,10,12,12a-tetrahydroxy-1,11-dioxo-2-tetracenecarboxamide 2.3g, yield: 79.3%.
[0144] 4. Preparation method Referring to step 4 in Example 1, cast [S-(4α, 12aα)]-9-[2-(N,N-diethylamino)-acetamido]-4,7-bis( Dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,10,12,12a-tetrahydroxy-1,11-dioxo-2-tetracene Amide...
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