HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium tri-s-butylborohydride → HCID 86640807, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium tri-s-butylborohydride | HCID 3611392 | — |
| Reactant | HCID 87126742 | HCID 87126742 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86640807 | HCID 86640807 | — |
Reaction Steps
To a chilled (−78° C.) solution of 2-methyl-propane-2-sulfinic acid [1-(2-bromo-pyridin-4-yl)-eth-(E)-ylidene]-amide (9.3 g, 31 mmol) in THF (280 mL) was added a 1 M solution of L-Selectride in THF (61.3 ml, 61.3 mmol) dropwise. After 2.5 hours, the chilled mixture was quenched with saturated aqueous NH4Cl (100 mL). The layers were separated and the aqueous layer was extracted with EtOAc (2×400 mL). The combined organic layers were washed with brine, and concentrated. The residue was purified by silica gel chromatography eluting with a gradient of 50-90% EtOAc in hexanes to afford 2-methyl-propane-2-sulfinic acid [(S)-1-(2-bromo-pyridin-4-yl)-ethyl]amide as a light yellow oil which contained 5% of the opposite diastereomer.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07879873B2 |
| Source dataset | uspto-grants-2011_02 |
| ORD ID | ord-e473a7143b334b099d5295d627c2a15b |
| Source note | uspto-grants-2011_02 |