HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tributylstannane → 1-(3,3-Dimethyl-2,3-dihydro-benzofuran-5-yl)-cyclopropanecarboxylic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tributylstannane | HCID 5948 | — |
| Reactant | Azobisisobutyronitrile | HCID 6547 | — |
| Reactant | 1-[3,5-Diiodo-4-(2-methyl-allyloxy)-phenyl]cyclopropane-carboxylic acid methyl ester | HCID 59129218 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 1-(3,3-Dimethyl-2,3-dihydro-benzofuran-5-yl)-cyclopropanecarboxylic acid methyl ester | HCID 59129355 | 62% |
Reaction Steps
To a solution of 1-[3,5-diiodo-4-(2-methyl-allyloxy)-phenyl]-cyclopropane-carboxylic acid methyl ester (3.5 g, 7.0 mmol) in toluene (15 mL) was added Bu3SnH (2.4 g, 8.4 mmol) and AIBN (0.1 g, 0.7 mmol). The mixture was heated at reflux overnight. The reaction mixture was concentrated under vacuum and the residue was purified by column chromatography on silica gel (petroleum ether/ethyl acetate 20:1) to give 1-(3,3-dimethyl-2,3-dihydro-benzofuran-5-yl)-cyclopropanecarboxylic acid methyl ester (1.05 g, 62%). 1H NMR (400 MHz, CDCl3) δ 7.10-7.07 (m, 2H), 6.71 (d, J=8 Hz, 1H), 4.23 (s, 2H), 3.62 (s, 3H), 1.58-1.54 (m, 2H), 1.34 (s, 6H), 1.17-1.12 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07776905B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-beb114265cc944cebfd63b9cb1601931 |
| Source note | uspto-grants-2010_08 |