HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → Methyl 5-bromo-3-(tetrahydro-2H-thiopyran-4-yl)-1H-indole-7-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Triethylsilane | HCID 12052 | — |
| Reactant | Trimethylsilyl triflate | HCID 65367 | — |
| Reactant | Tetrahydrothiopyran-4-one | HCID 66173 | — |
| Reactant | Ethyl 5-bromo-1H-indole-7-carboxylate | HCID 59332585 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Methyl 5-bromo-3-(tetrahydro-2H-thiopyran-4-yl)-1H-indole-7-carboxylate | HCID 59332577 | 76.1% |
Reaction Steps
TMSOTf (2.1 mL, 11.8 mmol) was added dropwise over 2.25 min to a solution of tetrahydro-4H-thiopyran-4-one (0.686 g, 5.9 mmol) in DCM (75 mL) at 0° C. (bath temp). A solution of ethyl 5-bromo-1H-indole-7-carboxylate (1.5 g, 5.9 mmol) in DCM (25 mL) was added dropwise via addition funnel over 20 min. Triethylsilane (3.76 mL, 23.6 mmol) was added in one portion and the reaction was allowed to warm to room temperature over 15 h. Saturated aqueous Na2CO3 (35 mL) was added, the layers were separated and the aqueous layer was extracted with DCM (1×75 mL). The combined organic layers were concentrated under reduced pressure, the crude product was washed with MeOH (2×8 mL) and dried under high vacuum, giving 1.59 g (76%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08071584B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-986cba858af349019cafa5cb659e245a |
| Source note | uspto-grants-2011_12 |