HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 68679919, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | HCID 11547106 | HCID 11547106 | — |
| Reactant | HCID 86602832 | HCID 86602832 | — |
| Reactant | HCID 178418573 | HCID 178418573 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 68679919 | HCID 68679919 | — |
Reaction Steps
To a solution of (R)-1-(2-(1-(3,4-dichlorophenylsulfonyl)-3-oxo-1,2,3,4-tetrahydropyrazin-2-yl)acetyl)azepan-4-one (4) (0.0250 g, 0.054 mmol) in THF (8.00 ml, 0.054 mmol) under N2 was added methylmagnesium bromide (1.4M solution in THF/Toluene (75:25), 2.70 ml, 3.78 mmol) in thee times, and stirred overnight. The reaction mixture was cooled in ice-water bath and sodium sulfate dodecahydrate (10.0 g) was added slowly followed by AcOEt (20 ml). After stirring at r.t. for 1 h, the mixture was filtered and the solid was washed with AcOEt. The filtrate was concentrated under reduced pressure and the crude product was chomatographed on silica (CH2Cl2→CH2Cl2/MeOH=20/1) to yield the product. MS 476 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07662811B2 |
| Source dataset | uspto-grants-2010_02 |
| ORD ID | ord-5af5cbf265294be385099210fb690901 |
| Source note | uspto-grants-2010_02 |