HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,4-Dinitrobenzoic acid → HCID 86740136, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,4-Dinitrobenzoic acid | HCID 10709 | — |
| Reactant | Dicyclohexylcarbodiimide | HCID 10868 | — |
| Reactant | Deacetyldiltiazem | HCID 91638 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86740136 | HCID 86740136 | 43.8% |
Reaction Steps
1.2 g of (+)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-[2-(dimethylamino)ethyl]-2,3-dihydro-1,5-benzothiazepin-4(5H)-one, 1.16 g of 3,4-dinitrobenzoic acid and 0.76 g of dicyclohexylcarbodiimide are dissolved in 20 ml of methylene chloride, and the solution is stirred at room temperature overnight. After the reaction, the precipitates are collected by filtration. The filtrate is washed with water, dried and then evaporated to remove solvent. The residue is purified by silica gel chromatography (solvent, chloroform:methanol=100:3), whereby 0.8 g of (+)-cis-2-(4-methoxyphenyl)-3-(3,4-dinitrobenzoyloxy)-5-[2-(dimethylamino)ethyl]-2,3-dihydro-1,5-benzothiazepin-4(5H)-one is obtained as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04521430 |
| Source dataset | uspto-grants-1985_06 |
| ORD ID | ord-ff775064af18435483cd506eb87e1229 |
| Source note | uspto-grants-1985_06 |