HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → Trifluoroacetic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 3,4,5-Trifluorobenzyl alcohol | HCID 2777040 | — |
| Reactant | HCID 86676392 | HCID 86676392 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Trifluoroacetic acid | HCID 6422 | 11.42% |
| Product | HCID 71236712 | HCID 71236712 | — |
Reaction Steps
To a solution of NaH (38.3 mg, 0.956 mmol) in DMF (2 mL) was added (3,4,5-trifluorophenyl)methanol (65 mg, 0.401 mmol) at rt. The reaction mixture was stirred for 5 mins at rt, and then 8-chloro-1-methyl-3,4-dihydro-1H-pyrimido[1,6-a]pyrimidin-6(2H)-one trifluoroacetic acid salt (100 mg, 0.319 mmol) was added. The reaction mixture was stirred for another 1 h at rt, quenched with water and then filtered to give clear solution. The solution was purified by MDAP (0.3% TFA in water/MeCN) to afford the title compound as its TFA salt (16 mg, 0.036 mmol, 11.42%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09273054B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-b0dd83b5ba854cc2b7df1f05e94c5839 |
| Source note | uspto-grants-2016_03 |