huagongshe.com
HRID1455557

反应详情

EQUATION

反应方程式

HRID 1455557 的结构方程式

REACTANTS

反应物

3
结构：CCN(C(C)C)C(C)C
HCID81531

Diisopropylethylamine

C8H19N

结构：NS(=O)(=O)c1c(Cl)sc(Cl)c1Br
HCID2740318

未命名化合物

结构：CC(C)(C)OC(=O)N1C2CCC1CC(=C(C#N)C(=O)O)C2
HCID68443024

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)(C)OC(=O)N1C2CCC1CC(=C(C#N)C(=O)NS(=O)(=O)c1c(Cl)sc(Cl)c1Br)C2
HCID68443476

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

3
结构：CN(C)c1ccncc1
催化剂HCID14284

N,N-Dimethylpyridin-4-amine

C7H10N2

结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

结构：CC(=O)N(C)C
溶剂HCID31374

Dimethylacetamide

C4H9NO

PROCEDURE

实验过程

120 μl of DIEA are added to a solution of 102 mg of 3-(carboxy-cyano-methylene)-8-aza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester, 162 mg of 4-bromo-2,5-dichloro-thiophene-3-sulfonamide, 583 μl of PPA in DMF (50%) and 43 mg of DMAP in 4 ml of DMA, and the mixture obtained is stirred at RT for 48 hours. From the mixture obtained solvent is removed in vacuo and the residue obtained is subjected to preparative HPLC on an RP-18 column. 3-[2-(4-Bromo-2,5-dichloro-thiophene-3-sulfonylamino)-1-cyano-2-oxo-ethylidene]-8-aza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester in the form of a foam is obtained.

WORKUP

后处理

  1. customFrom the mixture obtained solvent
  2. customis removed in vacuo
  3. customthe residue obtained