HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromotrimethylsilane → HCID 178457729, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromotrimethylsilane | HCID 76113 | — |
| Reactant | HCID 178476956 | HCID 178476956 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178457729 | HCID 178457729 | — |
Reaction Steps
To a solution of diethyl 4-(5-(2-(4-hydroxy-2-(pyridazin-3-yl)pyrimidine-5-carboxamido) propan-2-yl)pyridin-2-yl)phenylphosphonate (180 mg, 0.33 mmol) in DCM (5 ml) was added dropwise TMSBr (1.50 g, 9.85 mmol) at 0° C., the reaction mixture was stirred at room temperature for overnight. Then evaporated the solution and diluted with 20 ml MeOH, and stirred at room temperature for 30 mins, concentrated under vacuo, purified by Pre-HPLC to give product 33-1. 1H NMR (CDCl3-d6, 300 MHz,): δ 9.50 (s, 1H), 8.71 (s, 1H), 8.50 (d, 1H), 8.11 (m, 2H), 7.72-8.02 (m, 5H), 3.15 (s, 1H), 1.76 (s, 6H). (M+H)+=493.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09079930B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-1ebf8ff204cc4c409aeb37644098d93f |
| Source note | uspto-grants-2015_07 |