Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Benzyl carbamate | HCID 12136 | — |
| Reactant | Bismuth nitrate pentahydrate | HCID 160911 | — |
| Reactant | 5-(Prop-2-en-1-yl)cyclopent-2-en-1-one | HCID 13444545 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Benzyl 3-allyl-4-oxocyclopentylcarbamate | HCID 67513633 | — |
Reaction Steps
A solution of 5-(propene-3-yl)cyclopent-2-enone (4.28 g, 35 mmol) in dichloromethane (15 mL) was treated with benzyl carbamate (10.6 g, 70 mmol) and bismuth trinitrate pentahydrate (2.2 g, 4.5 mmol), stirred rapidly for 18 h, then diluted with dichloromethane (50 mL). The mixture was filtered through Celite® (rinse with dichloromethane) and the filtrate added directly to a silica gel column (˜550 cc). Elution first with 3:2 petroleum ether/dichloromethane afforded recovered starting material (1.01 g), then 4:1 heptane/ethyl acetate gave the subject compound (4.54 g, 47.5% uncorrected yield) as a pale yellow oil. NMR (CDCl3): δ 7.28 (br s, 5 H), 5.55-5.70 (m, 1 H), 5.03 (br s, 2 H), 4.90-5.10 (m, 2 H), 4.75-4.90 (m, 1 H), 4.10-4.30 (m, 1 H), 2.40-2.80 (m, 2 H), 2.15-2.40 (m, 2 H), 1.85-2.15 (m, 3 H). MS (M+Na): 296.0; MS (M−H2O+1): 256.0 (no M+1 visible).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09440995B2 |
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| Source dataset | uspto-grants-2016_09 |
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| ORD ID | ord-f2d56955c2bc4d60b6aa20377463e990 |
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| Source note | uspto-grants-2016_09 |
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