HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → Ethyl 1-chloroisoquinoline-7-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-Chloroisoquinoline-7-carbonyl chloride | HCID 87420700 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Ethyl 1-chloroisoquinoline-7-carboxylate | HCID 86664617 | 96% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
1-Chloroisoquinoline-7-carbonyl chloride (3.02 g, 13.4 mmol) was dissolved in tetrahydrofuran (135 mL) and was cooled to 0° C. Ethanol (6.1 mL, 94 mmol) and triethylamine (2.05 mL, 14.7 mmol) were added. The reaction was allowed to warm to room temperature and stir for 2 hours. The reaction mixture was partitioned between ethyl acetate (500 mL) and saturated aqueous sodium bicarbonate (250 mL). The organic layer was dried over magnesium sulfate, filtered, and concentrated to give the title compound (3.0 g, 96%) as a yellow solid. +ESI (M+H) 236.1; 1H NMR (400 MHz, CDCl3, δ): 9.06 (s, 1H), 8.30-8.39 (m, 2H), 7.89 (d, J=8.6 Hz, 1H), 7.63 (d, J=5.7 Hz, 1H), 4.48 (q, J=7.1 Hz, 2H), 1.46 (t, J=7.1 Hz, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08993586B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-fac4407511e84e1d8e5a7f3d1d8c50cb |
| Source note | uspto-grants-2015_03 |