Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 70100453 | HCID 70100453 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 21184439 | HCID 21184439 | — |
Reaction Steps
Formic acid[ethoxy-(6,6-dimethyl-3-methylthio-4-oxo-4,5,6,7-tetrahydrobenzo[c]thiophen-1-yl)methylene]hydrazide (150 mg, 0.49 mmol) was dissolved in a solution of methylamine in ethanol (30%, 10 mL) and the mixture heated at 60° C. More methylamine solution (10 mL) was added periodically over 8 h. The solution was evaporated to dryness and the residue purified by chromatographed on silica gel, eluting with methanol:dichloromethane (5:95). The title compound was obtained as a white powder (60 mg, 44%). mp 178-180° C. Found: C, 52.50; H, 5.43; N, 12.73%. C14H17N3OS2.0.8 (H2O) requires: C, 52.25; H, 5.83; N, 13.06%. 1HNMR (360 MHz, CDCl3)δ 1.05 (6H, s), 2.44 (2H, s), 2.62 (3H, s), 2.79 (2H, s), 3.75 (3H, s), 8.28 (1H, s). MS (ES+) 308 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06262103B1 |
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| Source dataset | uspto-grants-2001_07 |
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| ORD ID | ord-a3b2b77f36364482a0f27138e37d8c59 |
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| Source note | uspto-grants-2001_07 |
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