HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 58504033, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 58503934 | HCID 58503934 | — |
| Reactant | HCID 178418573 | HCID 178418573 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58504033 | HCID 58504033 | 32.1% |
Reaction Steps
To a solution of the compound prepared in Example 363 (0.112 g) in tetrahydrofuran (3 mL) at 0° C. was added a 3.0 M solution of methylmagnesium bromide in diethyl ether (0.27 mL), and the reaction mixture was stirred at room temperature for 3 hours. The reaction mixture was poured onto cold saturated ammonium chloride, and the mixture was extracted with ethyl acetate. The combined organics were washed with brine, dried over magnesium sulfate and concentrated. The residue was purified by column chromatography on silica gel (ethyl acetate:hexanes:triethylamine=80:20:1) to obtain the title compound (0.035 g) having the following physical data.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08809538B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-b04c5e073dad4d2e93dc0677bc63d73a |
| Source note | uspto-grants-2014_08 |