HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 68110255, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 68109751 | HCID 68109751 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68110255 | HCID 68110255 | 88% |
Reaction Steps
Excess hydrogen chloride gas was bubbled into a solution of tert-butyl N-[(1-[6-ethylthieno[2,3-d]pyrimidin-4-yl]piperidin-4-yl)methyl]carbamate (3.4 g, 9.03 mmol, 1.00 equiv) in dichloromethane (30 mL). The resulting solution was stirred for 2 h at room temperature. The product was precipitated and collected by filtration. The solid was dried in an oven under reduced pressure to give 2.5 g (88%) of Compound I-178 as a yellow solid. 1H NMR: (400 MHz, CD3OD) δ 8.59 (1H, s), 7.46 (1H, s), 4.90-4.95 (2H, d), 3.44-3.50 (2H, t), 3.02-3.07 (2H, q), 2.94-2.95 (2H, d), 2.16-2.21 (1H, m), 2.06-2.09 (2H, d), 1.49-1.55 (2H, q), 1.39-1.43 (3H, t). MS: m/z 277 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09340554B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-6873f2fb4777452bbb789d29027c02ec |
| Source note | uspto-grants-2016_05 |