HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 68313816, compound → HCID 53241571, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 68313816 | HCID 68313816 | — |
| Solvent | Trifluoroacetic acid methylene chloride | HCID 21863450 | — |
| Product | HCID 53241571 | HCID 53241571 | 53% |
Reaction Steps
A solution of the carbamate (8) (28 mg, 0.04 mmol) in DCM/TFA (1:1 v/v, 2.0 mL) was stirred at RT for 30 min. The reaction mixture was evaporated in vacuo and the resulting residue was subjected to capture and release on SCX and then triturated from diethyl ether (10 mL) to afford the title compound (Example 10) as an off-white solid (13 mg, 53%): m/z 634 (M+H)+ (ES+). 1H NMR (400 MHz, DMSO-d6) δ: 1.26 (9H, s), 2.39 (3H, s), 2.73-2.92 (3H, overlapping m), 3.56-3.64 (4H, overlapping m), 3.82 (1H, m), 5.38 (2H, s), 6.35 (1H, s), 7.00 (1H, d), 7.29 (1H, dd), 7.36 (2H, m), 7.44 (2H, m), 7.58-7.62 (3H, overlapping m), 7.92 (1H, m), 8.28-8.35 (3H, overlapping m), 8.58 (1H, br s), 8.79 (1H, br s), 10.09 (1H, br s) [partial assignment].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08299073B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-729744bf67f3462e8d063b93a2e0ad1b |
| Source note | uspto-grants-2012_10 |