Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Dichloromethane ethylacetate | HCID 21226138 | — |
| Reactant | HCID 123569579 | HCID 123569579 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 46945559 | HCID 46945559 | 76% |
Reaction Steps
A solution of HCl in ethyl ether (2N, 3 ml) is added in 31-ml portions to a solution of Example 29 (250 mg, 0.36 mmole) in a CH2Cl2/AcOEt mixture (5 ml/3 ml) cooled down to 0° C., and the mixture is stirred for 60 hours at 23° C. The volatiles are evaporated off under vacuum and the residue is taken up in a CH2Cl2 (50 ml) and NaHCO3 (50 ml) mixture. After stirring and decantation, the organic phase is washed with water (50 ml) followed by salt water. After drying over Na2SO4, filtration and concentration to dryness, the residue is purified on a silica column (Heptane/AcOEt:10/0 to 1/1). The expected product is obtained in the form of a white solid with a yield of 76%. Melting point: 102-104° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08710091B2 |
|---|
| Source dataset | uspto-grants-2014_04 |
|---|
| ORD ID | ord-77e5e8f591b04f6985924204104dd802 |
|---|
| Source note | uspto-grants-2014_04 |
|---|