HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 70913855, compound → HCID 70913850, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 70913855 | HCID 70913855 | — |
| Reactant | HCID 178418689 | HCID 178418689 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 70913850 | HCID 70913850 | 24% |
Reaction Steps
To a stirred solution of compound 36 (86 mg, 0.19 mmol) in dry THF (2 mL) was added CH3MgBr (3M, 70 μL, 0.21 mmol) and the mixture was stirred at rt for 2 h, quenched with aq. NH4Cl at 0° C. and extracted with EA. The organic layer was concentrated and purified by CC (PE/EE=4/1) to give compound 37 (21 mg, 24%) as a colorless solid. 1H-NMR (CDCl3+D2O, 400 MHz) δ: 0.67-0.72 (2H, m), 0.88-0.91 (2H, m), 1.01-1.05 (5H, m), 1.36-1.44 (3H, m), 1.60 (9H, m), 1.93-1.95 (2H, t, J=10.4 Hz), 2.52 (3H, s), 3.63-3.65 (2H, d, J=7.2 Hz), 4.43-4.45 (2H, t, J=10.4 Hz), 6.35 (1H, s), 6.49 (1H, s), 6.98 (1H, s). MS Calcd.: 472; MS Found: 473 (M+1)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08946446B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-f50c6ca3e1304a9f882e1ab544b7936b |
| Source note | uspto-grants-2015_02 |