HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 87279479, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | Benzyl 9-oxo-3-azaspiro[5.5]undecane-3-carboxylate | HCID 59803011 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 87279479 | HCID 87279479 | — |
Reaction Steps
Phosphorus oxychloride (5.68 mL) was added dropwise to a cooled (0° C.) solution of EXAMPLE 391D (18.37 g) in N,N-dimethylformamide (20 mL) and dichloromethane (80 mL). The mixture was then stirred overnight before it was diluted with ethyl acetate (600 mL) and washed with aqueous sodium acetate, water (3×), and brine and dried over Na2SO4. After filtration and concentration, the crude product was used directly in the next reaction without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09029404B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-643738a70c464eb8bb6fc652b2ce8dd5 |
| Source note | uspto-grants-2015_05 |