HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 8-[5-({[2-Amino-5-(2-thienyl)phenyl]amino}carbonyl)pyridin-2-yl]-N-ethyl-1,8-diazaspiro[4.5]decane-1-carboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | tert-Butyl 2-(6-chloronicotinamido)-4-(thiophen-2-yl)phenylcarbamate | HCID 57717453 | — |
| Reactant | n-Ethyl-1,8-diazaspiro[4.5]decane-1-carboxamide | HCID 57717467 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | 8-[5-({[2-Amino-5-(2-thienyl)phenyl]amino}carbonyl)pyridin-2-yl]-N-ethyl-1,8-diazaspiro[4.5]decane-1-carboxamide | HCID 24745117 | — |
Reaction Steps
A solution of intermediate F (82 mg, 0.19 mmol), N-ethyl-1,8-diazaspiro[4.5]-decane-1-carboxamide (73 mg, 0.35 mmol), and NEt3 (43 μL, 0.31 mmol) in 5 mL of DMSO was stirred at 90° C. for 12 h. The reaction mixture was partitioned between EtOAc and saturated NaHCO3, the organic layer was dried (MgSO4), filtered and concentrated. The residue was stirred in 2 mL of TFA and 2 mL of CH2Cl2 for 1 h at room temperature and concentrated. Reverse-phase chromatography (10 to 100% MeCN/water with 0.05% TFA) followed by neutralization with EtOAc/saturated NaHCO3 extraction and drying with MgSO4 gave the title compound: MS (ESI+): cal'd [M+H]+ 505.2, obs'd 505.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07544695B2 |
| Source dataset | uspto-grants-2009_06 |
| ORD ID | ord-a68fd1780a1f4e818f367a7d8b246fa7 |
| Source note | uspto-grants-2009_06 |