HuagongsheHuagongshe Chemistry Print Report · For research reference only
Vinyl chloroformate → HCID 59694179, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Vinyl chloroformate | HCID 78808 | — |
| Reactant | (1-Benzylpyrrolidin-3-yl)methanol | HCID 5176654 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 59694179 | HCID 59694179 | 71% |
Reaction Steps
A solution of (1-benzyl-pyrrolidin-3-yl)-methanol (prepared as described by Y.-H. Wu and R. F. Feldkamp, Pyrrolidines I, 1961, 26, 1519-1524) (455 mg, 2.38 mmol) and vinyl chloroformate (0.40 mL, 4.7 mmol) in 1,2-dichloroethane (10 mL) was heated to reflux for 2 h then concentrated in vacuo. Purification of the crude material by column chromatography on silica gel (5% MeOH/CH2Cl2) gave a yellow oil (440 mg, 71%). 1H NMR (CDCl3) δ 1.84 (m, 1H), 2.26 (m, 1H), 3.03 (m, 5H), 4.01 (br s, 2H), 4.23 (m, 2H), 4.61 (dd, 1H, J=6.2, 2.3 Hz), 4.93 (dd, 1H, J=14, 2.1 Hz), 7.06 (dd, 1H, J=14, 6.3 Hz), 7.41 (m, 3H), 7.53 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07354932B2 |
| Source dataset | uspto-grants-2008_04 |
| ORD ID | ord-239ef321e49743969e7c49d431852c8c |
| Source note | uspto-grants-2008_04 |