Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 59467884 | HCID 59467884 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 68511847 | HCID 68511847 | 77% |
Reaction Steps
Compound 69 (162 mg, 4.7 mmol) was dissolved in 10 mL of Et2O and 2.5 mL of EtOH, stirred for 10 min, then 0.57 mL of 1M HCl (in Et2O) was added slowly. The precipitation started upon addition of the acid. The reaction mixture was stirred for 1 h at RT, 40 min at 0° C., filtered. The precipitate washed with Et2O and dried under high vacuum over P4O10 overnight, then at 45° C. for 4 h to yield compound 70 (150 mg, 77%): MS: m/z+ 342.1 (M+H)+; Anal. Calcd (found) for C17H16ClN3OS2: C, 54.03 (53.78); H, 4.27 (4.33); N, 11.12 (10.95); Cl, 9.38 (9.15); S, 16.97 (16.68).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08916550B2 |
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| Source dataset | uspto-grants-2014_12 |
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| ORD ID | ord-de419a28b3be46359dd805965f4c6d14 |
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| Source note | uspto-grants-2014_12 |
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