HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Sulfate → HCID 89543564, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Sulfate | HCID 24436 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 89543728 | HCID 89543728 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 89543564 | HCID 89543564 | 75% |
Reaction Steps
A solution of 6-cyclopropylthiomorpholin-3-one (4-13, 355 mg, 2.258 mmol) in THF (10 ml) was cooled to 0° C. To this was added 2M LAH (2.3 ml, 4.60 mmol) slowly. After the addition was complete the cooling bath was removed and the mixture allowed to warm to rt. After stirring overnight the mixture was cooled to 0° C. and slowly quenched with 2M NaOH until gas evolution had ceased and a fine white precipitate formed. Anhydrous Na2SO4 was added and the mixture stirred for 15 minutes. The slurry was filtered through a pad of Celite washing with THF and the filtrate concentrated to afford 2-cyclopropylthiomorpholine (4-14, 242 mg, 75%) as a pale yellow oil which was used in subsequent steps as is.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09278960B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-06ed3f94c7d64b27827299239f0e3200 |
| Source note | uspto-grants-2016_03 |