HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetone → (2e)-3-(4-Amino-3-bromothieno[3,2-c]pyridin-7-yl)acrylaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetone | HCID 180 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | 3-Bromo-7-[(1e)-3,3-diethoxy-1-propenyl]thieno[3,2-c]pyridin-4-amine | HCID 18450774 | — |
| Solvent | Water | HCID 962 | — |
| Product | (2e)-3-(4-Amino-3-bromothieno[3,2-c]pyridin-7-yl)acrylaldehyde | HCID 18450636 | 164.3% |
Reaction Steps
A mixture of Example 176A (200 mg, 0.56 mmol), p-toluenesulfonic acid (10 mg), acetone (10 mL), and water (1 mL) at ambient temperature was stirred for 16 hours. The mixture was concentrated and washed with sodium bicarbonate (12 mL). The aqueous layer was extracted with dichloromethane/methanol (9:1). The combined organic extracts were concentrated to provide the desired product (160 mg, 0.92 mmol). Reverse phase HPLC (5% to 95% acetonitrile over 25 minutes, 1 mL/min, 254 nm, hypersil HS 100 Å, C18, 5 μm, 250×4.6 column) Rt=15.5 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07737160B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-e9722cb53f9e4f5980965732bf189dbb |
| Source note | uspto-grants-2010_06 |