HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 57572489, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | L-Alanine, ethyl ester, hydrochloride (1:1) | HCID 2724356 | — |
| Reactant | HCID 57572464 | HCID 57572464 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 57572489 | HCID 57572489 | — |
Reaction Steps
To slurry of the 2-methoxy-TIAM-trithiazolide 5 (27.1 g, 0.05 mol) and triethylamine (2 mL) in dichloromethane (600 mL), a solution of □-alanine ethyl ester HCl salt (1.1 g, 7 mmol) in DMF (15 mL) and dichloromethane (100 mL) was added dropwise over 36 h. The reaction mixture was applied directly onto a gradient flash silica column (1-3% methanol in dichloromethane). The desired product was obtained as thick, yellow oil. Yield 2.3 g (61% based on the □-alanine ethyl ester HCl salt).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08551453B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-5c5ff42fc7434cdab4df2bea8fb5cffd |
| Source note | uspto-grants-2013_10 |