HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzenecarbothioic acid, 2,5-difluoro-, hydrazide → HCID 68507256, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzenecarbothioic acid, 2,5-difluoro-, hydrazide | HCID 55279024 | — |
| Reactant | HCID 68503911 | HCID 68503911 | — |
| Solvent | Dichloromethane ethanol | HCID 21584144 | — |
| Product | HCID 68507256 | HCID 68507256 | 87% |
Reaction Steps
To a solution of tert-butyl 4-(3-(tert-butyldimethylsilyloxy)phenyl)-4-oxobutylcarbamate (1.400 g, 3.55 mmol) in 20 mL of a 3:1 EtOH/DCM mixture was added 2,5-difluorobenzothiohydrazide (0.704 g, 3.74 mmol). The reaction was stirred overnight at room temperature, then heated to 45° C. for 10 hours. The reaction mixture was then concentrated in vacuo, loaded directly to Biotage (45), followed by flash column chromatography (20-50% ethyl acetate/hexanes), yielding the desired product as a yellow semi-solid (1.742 g, 82%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07795282B2 |
| Source dataset | uspto-grants-2010_09 |
| ORD ID | ord-778328ec231d4d38a42f00d2c58b3216 |
| Source note | uspto-grants-2010_09 |