HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 22478631, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Stannous Chloride | HCID 24479 | — |
| Reactant | HCID 22478944 | HCID 22478944 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 22478631 | HCID 22478631 | — |
Reaction Steps
A mixture of nitro compound 456a (593 mg; 2.83 mmol); SnCl2 (4.02 g; 20.8 mmol; 7.35 eq) and NH4OAc (4.5g) was suspended in THF:MeOH:H2O=1:1:1 (60 mL) and stirred at 70° C. for 2 h, cooled down, diluted with ethyl acetate and successively washed with saturated NaHCO3 and brine; dried (MgSO4) filtered and concentrated. The residue (443 mg; 2.43 mmol; 87%) showed consistent spectrum and suitable purity degree for synthetic purposes, therefore was submitted to the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07595343B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-f66df002e2c74b02bc9285b131559b95 |
| Source note | uspto-grants-2009_09 |