HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → (R)-(-)-1-CBZ-3-pyrrolidinol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Benzyl chloroformate | HCID 10387 | — |
| Reactant | (R)-3-Pyrrolidinol | HCID 2759337 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (R)-(-)-1-CBZ-3-pyrrolidinol | HCID 11183628 | 62% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
3-Hydroxy-(R)-pyrrolidine (8.71 g, 0.1 mol) was dissolved in CH2Cl2 (260 mL) and cooled to 0° C. Triethylamine (33.5 mL, 0.24 mol) and benzyl chloroformate (14.9 mL, 0.11 mol) were added, and the resulting solution was stirred for 2 h at 0° C. The solution was gradually warmed to room temperature and allowed to stir overnight. The solution was washed with 1 M HCl, saturated NaHCO3, and brine. The organic solution was dried over MgSO4 and concentrated. The crude product was purified by column chromatography eluting with ethyl acetate to afford 13.7 g (62% yield, 2 steps) of the desired product as a purple oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06914048B2 |
| Source dataset | uspto-grants-2005_07 |
| ORD ID | ord-10cba454024346c69c6ee226f2ea5054 |
| Source note | uspto-grants-2005_07 |