HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 59835738, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Stannous chloride dihydrate | HCID 61436 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 10049301 | HCID 10049301 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 59835738 | HCID 59835738 | — |
Reaction Steps
200 mg (2.5 mmol) NaHCO3 and 300 mg (1.1 mmol) tin-(II)-chloride dihydrate are added to a solution of 100 mg (0.22 mmol) 5-(4-chloro-phenyl)-2-[3-nitro-4-(2-pyrrolidin-1-yl-ethoxy)-phenylethynyl]-pyridine (Example 3.13) in 10 mL EtOAc and the reaction mixture is refluxed for 2 h. To complete the reaction a further 200 mg (2.5 mmol) NaHCO3, 300 mg (1.1 mmol) tin-(II)-chloride dihydrate and 1 mL MeOH are added and the mixture is refluxed for a further 2 h. After cooling, 4 g of silica gel are added, the solvent is eliminated i.vac. and the residue is purified by chromatography (silica gel, DCM/MeOH/NH3 8:2:0.2).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07452911B2 |
| Source dataset | uspto-grants-2008_11 |
| ORD ID | ord-df5fd63ed5954a5cbc001e1a9281a2b7 |
| Source note | uspto-grants-2008_11 |