HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → HCID 22313945, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | (Diethylamino)sulfur trifluoride | HCID 123472 | — |
| Reactant | HCID 10181629 | HCID 10181629 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22313945 | HCID 22313945 | 16% |
Reaction Steps
To 540 mg (11.37 mmol) 2-(Ethyl-{4-[3-(4-trifluoromethyl-phenyl)-benzo[d]isothiazol-6-yloxy]-butyl}-amino)-ethanol in 6 ml CH2Cl2 were added 0.22 ml (1.7 mmol) DAST at −78° C. After stirring at that temperature for 3.5 h, additional 0.2 ml (1.6 mmol) DAST were added and the mixture was slowly warmed to RT over night. The solution was added to a cooled aqueous solution of Na2CO3 and extracted with EtOAc. The organic phase was washed with brine and dried over Na2SO4. Column chromatography CH2Cl2:MeOH 95:5 yielded 79.3 mg (16%) Ethyl-(2-fluoro-ethyl)-{4-[3-(4-trifluoromethyl-phenyl)-benzo[d]isothiazol-6-yloxy]-butyl}-amine as brown oil, MS: 441 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07173043B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-e804b85aa7214365b582dc75ab0d88a5 |
| Source note | uspto-grants-2007_02 |