HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → beta-Hydroxy-ethyl 1,4-dihydro-2,6-dimethyl-3-nitro-4-(2-chlorophenyl)-pyridine-5-thiocarboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Mercapto-ethanol | HCID 4713212 | — |
| Reactant | 1,4-Dihydro-2,6-dimethyl-3-nitro-4-(2-chlorophenyl)-pyridine-5-carboxylic acid imidazolide | HCID 86741317 | — |
| Product | beta-Hydroxy-ethyl 1,4-dihydro-2,6-dimethyl-3-nitro-4-(2-chlorophenyl)-pyridine-5-thiocarboxylate | HCID 20216226 | — |
Reaction Steps
3 g of 1,4-dihydro-2,6-dimethyl-3-nitro-4-(2-chlorophenyl)-pyridine-5-carboxylic acid imidazolide are boiled in 12.5 ml of absolute tetrahydrofuran with 5 ml of mercaptoethanol for 7 hours. The mixture is concentrated, the concentrate is concentrated at 70° C. using an oil pump, the residue is dissolved in chloroform and the solution is washed twice with water, dried and concentrated. The resulting evaporation residue is purified over a silica gel column with a volume of 160 ml, using toluene and later toluene/ethyl acetate 6:1 as the mobile phase. 1.94 g of a yellow foam with an Rf value of 0.25 are obtained as the main fraction.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04645775 |
| Source dataset | uspto-grants-1987_02 |
| ORD ID | ord-a1da68f051494cb081b5b6e4331cbe71 |
| Source note | uspto-grants-1987_02 |