Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Thioanisole | HCID 7520 | — |
| Reactant | HCID 53629626 | HCID 53629626 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 59127130 | HCID 59127130 | 50.7% |
Reaction Steps
A solution of 3-[(1-methylethyl)oxy]-N-(3-methyl-1,2,4-thiadiazol-5-yl)-5-[(phenylmethyl)oxy]benzamide (33 g, 86 mmol), trifluoroacetic acid (160 mL) and thioanisole (50.5 mL) was stirred at ambient temperature for 48 hours. The TFA was removed in vacuo and the residue poured into saturated sodium bicarbonate solution (300 mL) and extracted into ethyl acetate (twice). The combined organic extracts were washed with brine, dried (MgSO4), filtered and the solvent removed in vacuo. The residue was triturated with DCM and washed with 5% ethyl acetate in isohexane to give the desired compound (12.8 g). 1H NMR δ (d6-DMSO): 1.31 (d, 6H), 2.51 (s, 3H), 4.67 (sept, 1H), 6.58 (s, 1H), 7.08 (s, 1H), 7.24 (s, 1H), 9.88 (s, 1H), 13.25 (brs, 1H). m/z 294 (M+H)+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07977328B2 |
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| Source dataset | uspto-grants-2011_07 |
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| ORD ID | ord-7690e8d5c8734224974f9d886122fb1c |
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| Source note | uspto-grants-2011_07 |
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