HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → HCID 67097069, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 59312361 | HCID 59312361 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 67097069 | HCID 67097069 | 90% |
Reaction Steps
A solution of methylamine (2.0M, 0.65 mL, 1.30 mmol) was added to a solution of Tert-butyl 2-(1-phenylethyl)-4-{[(trifluoromethyl)sulfonyl]oxy}-5,6,8,9-tetrahydro-7H-pyrimido[4,5-d]azepine-7-carboxylate of preparation 2, step B (130 mg, 0.26 mmol) in MeCN (4.0 mL) at room temperature with stirring. The mixture was stirred at room temperature for 20 h. The solvent was evaporated in vacuo to provide the crude title compound as a yellow gum. The crude material was purified by flash column chromatography eluting with CH2Cl2:ethyl acetate (100:0 to 50:50) to yield the desired product as a white crystalline solid (89 mg, 90% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07928099B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-caa837d02d5e48c78f9db47207937a6b |
| Source note | uspto-grants-2011_04 |