HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nipecotic Acid → HCID 11989748, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nipecotic Acid | HCID 4498 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 86621993 | HCID 86621993 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 11989748 | HCID 11989748 | 23% |
Reaction Steps
2′-Acetylamino-4′-methyl-[4,5′]bithiazolyl-2-carbonyl chloride, prepared as in Step I of Example 13, described above, (106.5 mg; 0.35 mmol; 1 eq.), is dissolved in THF (8 ml) and DCM (4 ml). Nipecotic acid (Emkachem)(42.8 mg; 0.33 mmol; 1 eq.) and triethylamine (97 μl; 0.70 mmol; 2 eq.) are added and the mixture is stirred overnight at rt. Solvents are evaporated and the crude product is crystallized in MeOH, filtrated, affording Compound (21) as a brown solid (31 mg; 23%). M− (ESI): 393; M+ (ESI): 395. HPLC (method A), Rt: 2.60 min (purity: 95.4%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07799814B2 |
| Source dataset | uspto-grants-2010_09 |
| ORD ID | ord-6726527b578046909ddbb157da4d0d5a |
| Source note | uspto-grants-2010_09 |