HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 66865062, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-[1-[(Methylsulfonyl)oxy]ethyl]-1-piperidinecarboxylic acid 1,1-dimethylethyl ester | HCID 23282886 | — |
| Reactant | HCID 66865178 | HCID 66865178 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 66865062 | HCID 66865062 | 90.1% |
Reaction Steps
To a 3-necked flask is added 1′-methanesulfonyl-1′,2′,3′,6′-tetrahydro-[2,4′]bipyridinyl-5-ol (254.3 g, 1.0 mol) followed by 4-(1-methanesulfonyloxy-ethyl)-piperidine-1-carboxylic acid tert-butyl ester (396.1 g,1.34 mol) and potassium carbonate (248.8 g, 1.8 mol). Dimethylformamide (3800 mL) is added and the mixture is heated at 80˜90° C. for 6 h. 3810 mL of water are added dropwise at 70˜80° C. The mixture is cooled slowly to 20˜30° C. and filtered. The cake is slurried with 1000 mL of water, concentrated and dried under vacuum to provide 407 g of a solid with 97.13% HPLC purity.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08207344B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-0c433fa4c48244708c65588633b55ae1 |
| Source note | uspto-grants-2012_06 |