HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Oxalic acid dihydrate → (2S)-5-[(benzyloxy)amino]-2-cyanopiperidine ethanedioate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Oxalic acid dihydrate | HCID 61373 | — |
| Edukt | (2S)-5-[(benzyloxy)amino]-2-cyanopiperidine | HCID 117599345 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Lösungsmittel | Ethylacetate acetone | HCID 21584569 | — |
| Produkt | (2S)-5-[(benzyloxy)amino]-2-cyanopiperidine ethanedioate | HCID 131732538 | 55% |
Reaktionsschritte
A solution of oxalic acid dihydrate (5.28 gm, 0.0418 mol) in a mixture of ethyl acetate: acetone (1:1, 28 ml:28 ml) was slowly added to a stirred solution of (2S)-5-[(benzyloxy)amino]-2-cyanopiperidine (X) (8.8 gm, 0.0380 mol, prepared according to the procedure described in step 7) in ethyl acetate (35 ml) at 25° C. After 3 hour of stirring, the separated solid was filtered under suction, washed with additional 50 ml of v/v mixture of ethyl acetate: acetone solution (1:1, 25 ml:25 ml) and the solid dried under reduced pressure to obtain 6.7 gm of (2S)-5-[(benzyloxy)amino]-2-cyanopiperidine ethanedioate (1:1) (XI) in 55% yield.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09115131B2 |
| Quelldatensatz | uspto-grants-2015_08 |
| ORD ID | ord-d2934f9d91be495da07054485c0fabaf |
| Quellennotiz | uspto-grants-2015_08 |