HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86670900, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 86670901 | HCID 86670901 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86670900 | HCID 86670900 | — |
Reaction Steps
To a fine suspension of ethyl 7-[(tert-butoxycarbonyl)amino]-1-(tetrahydro-2H-pyran-4-yl)-1,4-dihydropyrazolo[3′,4′:4,5]thiopyrano[3,2-d][1,3]thiazole-3-carboxylate 5,5-dioxide (182 mg; 0.37 mmol; 1.00 eq.) in DCM (540 μl) is added TFA (180 μl; 2.34 mmol; 6.40 eq.). The mixture is stirred at rt overnight after which water is added to the reaction mixture. The precipitate is washed with water then dried under vacuum to afford the title compound as an off-white powder. 1H NMR (DMSO) δ 8.34 (bs, 2H), 5.61-5.43 (m, 1H), 4.91 (s, 2H), 4.33 (q, J=7.1 Hz, 2H), 4.12-3.93 (m, 2H), 3.52-3.35 (m, 2H), 3.20-1.87 (m, 4H), 1.33 (t, J=7.1 Hz, 3H). HPLC (max plot) 95.1%; Rt 2.28 min. MS (ESI+): 398.7.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09073940B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-ca65454628a84583be0087764be7424e |
| Source note | uspto-grants-2015_07 |