HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trichloroacetyl isocyanate → (3R)-1-(t-butoxycarbonyl)-3-carbamoyloxypyrrolidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trichloroacetyl isocyanate | HCID 76400 | — |
| Reactant | tert-Butyl (3R)-3-hydroxypyrrolidine-1-carboxylate | HCID 6544479 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (3R)-1-(t-butoxycarbonyl)-3-carbamoyloxypyrrolidine | HCID 14254785 | 66.1% |
Reaction Steps
A solution of 4.52 g of trichloroacetyl isocyanate in 8 ml of methylene chloride was added to an ice-cooled solution of 3.75 g of (3R)-1-(t-butoxycarbonyl)-3-hydroxypyrrolidine in 40 ml of methylene chloride, and the mixture was stirred for 30 minutes with ice-cooling. After completion of the reaction, the solvent was stripped off from the reaction mixture and the residue was dissolved in 100 ml of methanol. The solution was stirred with 35 g of silica gel for 5 hours at 30° C., and then filtered. The filtrate was concentrated, giving 3.05 g of (3R)-1-(t-butoxycarbonyl)-3-carbamoyloxypyrrolidine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04771046 |
| Source dataset | uspto-grants-1988_09 |
| ORD ID | ord-1927cf25beb74e3c965c0dc7ca30daf1 |
| Source note | uspto-grants-1988_09 |