HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 56926093, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3,4-Dimethoxybenzenesulfonyl chloride | HCID 2734183 | — |
| Reactant | HCID 56926092 | HCID 56926092 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 56926093 | HCID 56926093 | 43% |
Reaction Steps
To a solution of 19a (20 mg, 0.075 mmol) in DCM (1 mL) was added 3,4-dimethoxybenzenesulfonyl chloride (36 mg, 0.150 mmol) and triethylamine (0.021 mL, 0.150 mmol). The reaction was stirred for 24 hours at room temperature. The reaction mixture was washed with water (×2) and the organic layer dried over MgSO4 and concentrated in vacuo. Column chromatography (2:1 hexane/EtOAc) gave a white solid (?? g). Yield: 43%. 1H NMR (CDCl3): δ 1.47 (s, 6H), 3.76 (s, 3H), 3.97 (s, 3H), 4.60 (s, 2H), 5.66 (d, 1H, J=9.6), 6.26 (d, 1H, J=10), 6.93-6.99 (m, 4H), 7.23-7.25 (m, 3H), 7.32-7.36 (m, 2H), 7.63 ppm (d, 1H, J=2.4). HRMS (ESI) m/z calcd for C25H25N2O5S [M+H)+] 467.1641. found: 467.1636. HPLC: ret. time=7.5 min, 99.0%
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09062072B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-4316f89118e34e0397c4d566cbdcdb73 |
| Source note | uspto-grants-2015_06 |