HuagongsheHuagongshe Chemistry Print Report · For research reference only
Vanillin → 4-[((3S)-1-tert-butoxycarbonyl-3-pyrrolidinyl)oxy]-3-methoxybenzaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Vanillin | HCID 1183 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | tert-Butyl (3R)-3-hydroxypyrrolidine-1-carboxylate | HCID 6544479 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4-[((3S)-1-tert-butoxycarbonyl-3-pyrrolidinyl)oxy]-3-methoxybenzaldehyde | HCID 57273622 | 77.9% |
Reaction Steps
In 50 ml of tetrahydrofuran were dissolved 3.04 g of vanillin, 3.74 g of (3R)-1-tert-butoxycarbonyl-3-hydroxypyrrolidine and 5.24 g of triphenylphosphine. The thus prepared solution was mixed with 4.00 g of diethyl azodicarboxylate, and the mixture was stirred at room temperature for 18 hours. After concentrating the resulting reaction solution, the thus obtained residue was purified by subjecting it to silica gel column chromatography using an ethanol/chloroform mixture as an elution solvent. In this way, 5.0 g of the title compound was obtained in an oily form.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05962695 |
| Source dataset | uspto-grants-1999_10 |
| ORD ID | ord-df34007fbbb34628be9a3504db89c733 |
| Source note | uspto-grants-1999_10 |