HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Fluorobenzothiohydrazide → Tert-butyl 3-(5-(3-fluorophenyl)-2-phenyl-2,3-dihydro-1,3,4-thiadiazol-2-yl)butylcarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Fluorobenzothiohydrazide | HCID 55281616 | — |
| Reactant | Tert-butyl 3-methyl-4-oxo-4-phenylbutylcarbamate | HCID 67214951 | — |
| Catalyst | Acetic Acid | HCID 176 | — |
| Solvent | Dichloromethane ethanol | HCID 21584144 | — |
| Product | Tert-butyl 3-(5-(3-fluorophenyl)-2-phenyl-2,3-dihydro-1,3,4-thiadiazol-2-yl)butylcarbamate | HCID 67215287 | 48.4% |
Reaction Steps
To a solution of 3-fluorobenzothiohydrazide (300 mg, 1.76 mmol) in ethanol/DCM (6 mL/2 mL) was added tert-butyl 3-methyl-4-oxo-4-phenylbutylcarbamate (538 mg, 1.94 mmol). After stirring at room temperature for 16 hours, acetic acid (3 drops) was added and the mixture stirred for another 48 hours. The reaction mixture was then concentrated under reduced pressure and chromatographed (9:1 hexanes/ethyl acetate) to provide the product (366 mg, 48%) as a mixture of diastereomers as a yellow foam.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08236825B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-9ff50a04ff16446f86147e267fe1ffdc |
| Source note | uspto-grants-2012_08 |