HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → HCID 67061210, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 2-Amino-5-bromo-3-pyridinecarbaldehyde | HCID 24213792 | — |
| Reactant | HCID 178418573 | HCID 178418573 | — |
| Product | HCID 67061210 | HCID 67061210 | 50% |
Reaction Steps
To a solution of 2-Amino-5-bromo-pyridine-3-carbaldehyde (632 mg, 3.14 mmol) in anhydrous THF (20 mL) was methylmagnesium bromide 3M in diethyl ether (6.06 mL, 34.8 mmol) is added at −50° C. The reaction mixture was warmed to room temperature and stirred overnight. Saturated aqueous ammonium chloride was added to the mixture (15 mL), the organic layer separated and the aqueous phase extracted with EtOAc (3×20 mL). Organic layers were dried over sodium sulfate, filtered and concentrated. The crude residue was purified by flash silica chromatography with a gradient of ethyl acetate in hexanes. (2-Amino-5-bromo-phenyl)-cyclopentyl-methanol (425.9 mg, 50% yield) was obtained as a yellow powder. MS: m/z 271/273[MH+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07582637B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-8b9fe0dd2f764763a09306f13cfa9a3c |
| Source note | uspto-grants-2009_09 |