HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 118223432, compound → HCID 118223433, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 118223432 | HCID 118223432 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 118223433 | HCID 118223433 | 55.3% |
Reaction Steps
Dissolve the crude product obtained in Step 3 (2.14 g, 4.7 mmol) in HCl solution in 1,4-dioxane (5 M, 10 mL). Stir the reaction at room temperature for 17 hrs. LC/MS shows reaction is complete. Remove the solvent under reduced pressure, suspend the solid in DCM and add carefully saturated NaHCO3 solution. Separate the organic layer. Extract the aqueous layer with DCM. Combine the organic layers, dry over anhydrous Na2SO4. Concentrate to give the crude product. Purification by chromatography (silica gel, EtOAc:PE=1:3) affords the title compound (0.9 g, 54% from step 2). MS: (M+1): 352.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09359338B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-f1771ed54bc843f3989dc7b05e998207 |
| Source note | uspto-grants-2016_06 |