HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyrrolidine → Bis(pyrrolidino)silacyclobutane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyrrolidine | HCID 31268 | — |
| Reactant | 1,1-Dichlorosilacyclobutane | HCID 75373 | — |
| Product | Bis(pyrrolidino)silacyclobutane | HCID 58385700 | 34% |
Reaction Steps
Bis(pyrrolidino)silacyclobutane was synthesized by reacting 1,1-dichlorosilacyclobutane with an excess amount of pyrrolidine (Equation 3). To do so, 23.7 ml (0.200 mol) 1,1-dichlorosilacyclobutane was added to 100.0 ml (1.20 mol) pyrrolidine in 1 L hexanes at −10° C. After bodying for two day at the room temperature, the reaction slurry was filtered to remove pyrrolidine hydrochloride salt. The filtrant was vacuum dried to give a liquid crude product which was then vacuum distilled. 15.4 g Product was isolated at 99.7% purity in 34% yield at 51° C. under 1 torr pressure. The structure of the product analyzed with 1H, 13C and 29Si NMR, FT-IR and GC-MS was in consistence with bis(pyrrolidino)silacyclobutane.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09117664B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-814981cf98f64db587b0d93590a00317 |
| Source note | uspto-grants-2015_08 |