HuagongsheHuagongshe Chemistry Print Report · For research reference only
Allyl bromide → Ethyl 4-(4-allyl-1,4-diazepan-1-yl)benzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Allyl bromide | HCID 7841 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Ethyl 4-(1,4-diazepan-1-yl)benzoate | HCID 18425301 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Ethyl 4-(4-allyl-1,4-diazepan-1-yl)benzoate | HCID 66589947 | 48.5% |
Reaction Steps
3-Bromoprop-1-ene (0.433 mL, 5.00 mmol) was added to a stirred solution of ethyl 4-(1,4-diazepan-1-yl)benzoate (1.242 g, 5 mmol) and DIPEA (2.183 mL, 12.50 mmol) in dichloromethane (20 mL). The reaction mixture was stirred under nitrogen at room temperature for 24 h. This was diluted with dichloromethane (20 mL), washed with water (2×25 ml) and saturated sodium chloride solution (20 ml), dried over MgSO4, filtered and evaporated to dryness. The crude product was purified by silica column chromatography, eluting with a gradient of 0 to 5% 2.5M ammonia/MeOH in DCM. Pure fractions were evaporated to dryness to afford ethyl 4-(4-allyl-1,4-diazepan-1-yl)benzoate (0.700 g, 48.5%) as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08129391B2 |
| Source dataset | uspto-grants-2012_03 |
| ORD ID | ord-4d4676441f7b407bb224031ccfb52456 |
| Source note | uspto-grants-2012_03 |