HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 53742729, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 57108817 | HCID 57108817 | — |
| Solvent | Water methylene chloride | HCID 21908982 | — |
| Product | HCID 53742729 | HCID 53742729 | 98% |
Reaction Steps
15.9 g (111 mmol) of the (2S*,5S*)-5-methylpiperidine-2-carboxylic acid described above was dissolved in 220 ml of a dichloromethane/water (1:1). 93.3 g (1.11 mol) of sodium hydrogencarbonate and 21.0 ml (222 mmol) of acetic anhydride were added thereto in this order at room temperature, followed by stirring for 3 days. The reaction solution was poured into 6N-hydrochloric acid under cooling with ice, and the extraction with chloroform was conducted. Then, the organic layer was dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated in a reduced pressure to give 20.1 g of the title compound as a colorless oil. Yield 98%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05789403 |
| Source dataset | uspto-grants-1998_08 |
| ORD ID | ord-01e78806deac4ab193ac740e3be59e49 |
| Source note | uspto-grants-1998_08 |