HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 131732144, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 562001 | HCID 562001 | — |
| Reactant | HCID 131732142 | HCID 131732142 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 131732144 | HCID 131732144 | — |
Reaction Steps
The mixture of Example 48D, (3-bromo-1-bromomethyl-propyl)-benzene (1.82 g, 5.9 mmol) and N,N-diisopropylethyl amine (2.1 g, 16.2 mmol) in acetonitrile (10 ml) was stirred at 120° C. in a microwave reactor for 2 hours. Water (15 mL) was added and extracted with ethyl acetate. The combined organics were dried and concentrated. The residue was purified by column chromatography (SiO2, petroleum ether: ethyl acetate from 50:1 to 10:1) to provide the title compound as an oil. 1H NMR (400 MHz, CDCl3) δ (ppm): 7.10-7.31 (m, 10H), 5.01-5.08 (s, 2H), 3.17 (d, 2H), 2.76 (q, 1H), 2.52-2.69 (m, 1H), 2.35-2.48 (m, 1H), 2.17-2.22 (m, 1H), 1.82-2.15 (m, 5H), 1.61-1.80 (m, 6H), 1.39-1.60 (m, 5H), 1.17-1.27 (m, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08906911B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-fbba6f7313f442c7aaf73b945799bd7b |
| Source note | uspto-grants-2014_12 |