HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → (2S)-5-[(benzyloxy)amino]-2-cyanopiperidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Reactant | (2S)-5-[(benzyloxy)imino]-2-cyanopiperidine | HCID 90088575 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | (2S)-5-[(benzyloxy)amino]-2-cyanopiperidine | HCID 117599345 | — |
Reaction Steps
The compound of Formula (IX) was reacted with sulphuric acid and sodium triacetoxy borohydride, in presence of suitable solvent such as ethyl acetate and at temperature below −5° C., to provide (2S)-5-[(benzyloxy)amino]-2-cyanopiperidine (X). The compound of Formula (X) was purified by forming oxalate salt. The compound of Formula (X) was reacted with oxalic acid in a mixture of ethylacetate and acetone to provide (2S)-5-[(benzyloxy)amino]-2-cyanopiperidine ethanedioate (1:1) (XI), which was further treated with sodium hydrogen carbonate to obtain purified (2S)-5-[(benzyloxy)amino]-2-cyanopiperidine (XII). The racemic compound (XI) was treated with methanol to obtain pure (2S,5R)-5-[(benzyloxy)amino]-2-cyanopiperidine ethanedioate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115131B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-6cc639d5d815446690f58645e01492a5 |
| Source note | uspto-grants-2015_08 |