HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 67498223, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | HCID 67496336 | HCID 67496336 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 67498223 | HCID 67498223 | 65.5% |
Reaction Steps
To a rt solution of 65.D (476 mg, 1.58 mmol) in EtOAc (9 mL) was added SnCl2-2H2O (1.88 g, 7.93 mmol). The reaction solution was refluxed for 2.0 hr, cooled to rt, and treated with concentrated NH4OH (2.5 mL). To the resulting mixture was added MeOH (10 mL) followed by celite. Solid was filtered off and washed with MeOH, the liquid layers was collected and concentrated. Purification of the residue by flash chromatography on silica gel using 0-20% MeOH/CH2Cl2 for elution gave title product 65.E as colorless syrup (282 mg, 65%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08785468B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-0fe26f0263a049e3bc5c8cd416d82925 |
| Source note | uspto-grants-2014_07 |