HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium borohydride → HCID 58514824, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 87228704 | HCID 87228704 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 58514824 | HCID 58514824 | 46.2% |
Reaction Steps
To a solution of example 10 (0.095 g, 0.259 mmol) in methanol (2 ml) cooled to 0° C., sodium borohydride (0.010 g, 0.259 mmol) was added and stirred for 1 h. The reaction was quenched by the addition of ice-cold water, extracted with ethyl acetate, washed with brine, dried over sodium sulphate and concentrated. The crude product was purified by column chromatography with methanol:dichloromethane to afford the title compound as an off-white solid (0.040 g, 46%). M.P.: 210-213° C. 1H-NMR (δ ppm, DMSO-d6, 400 MHz): 8.61 (d, J=8.7 Hz, 1H), 8.22 (d, J=8.3 Hz, 2H), 8.11 (d, J=8.8 Hz, 1H), 7.53 (m, 4H), 7.21 (m, 2H), 5.98 (s, 2H), 5.32 (t, J=5.8 Hz, 1H), 4.59 (d, J=5.7 Hz, 2H). MS (m/z): 335.05 (M++1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08481739B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-536872663fc945a09bf955e2d9c5bcb3 |
| Source note | uspto-grants-2013_07 |