HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 50923089, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 58292695 | HCID 58292695 | — |
| Solvent | Methanol tetrahydrofuran water | HCID 21892291 | — |
| Product | HCID 50923089 | HCID 50923089 | 27.8% |
Reaction Steps
The mixture of ethyl 2-(4-(aminomethyl)-1-hydroxy-6-methoxy-1,3-dihydrobenzo[c][1,2]oxaborol-3-yl)acetate (20 mg), LiOH (24 mg, 1 mmol) in THF/MeOH/H2O (1.5 ml/1.5 ml/1.5 ml) was stirred at room temperature for 2 hrs. The solvent was removed in reduced pressure to dryness. The crude product was purified by Prep-HPLC to give desired product 5 mg as white powder (TFA salt). 1H NMR (400 MHz, DMSO-d6) δ 9.27 (s, 1H), 8.22 (brs, 3H), 7.19 (d, J=2.4 Hz, 1H), 7.16 (d, J=2.4 Hz, 1H), 5.60 (dd, J=9.4, 2.2 Hz, 1H), 4.04 (q, J=4.5 Hz, 2H), 3.78 (s, 3H), 2.99 (dd, J=15.8, 2.4 Hz, 1H), and 2.11 (dd, J=9.4, 15.8 Hz, 1H). MS (ESI) m/z=252 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08343944B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-6a156f3037c841778ace9dc61b9d2c9c |
| Source note | uspto-grants-2013_01 |