Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cumylamine | HCID 68509 | — |
| Reactant | 3,6-Dichloro-4h-thieno[3,2-e][1,2,4]thiadiazine 1,1-dioxide | HCID 11832058 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178456997 | HCID 178456997 | 20% |
Reaction Steps
A solution of 3,6-dichloro-4H-thieno[3,2-e]-1,2,4-thiadiazine 1,1-dioxide (1.0 g, 3.9 mmol) and cumylamine (1.06 g, 7.8 mmol) in ethanol (6 ml) was stirred for 31 h at 120° C. in a sealed flask. The cooled solution was concentrated in vacuo and the residue dissolved in 1N sodium hydroxide (50 ml) followed by treatment with decolourising charcoal. After filtration, the clear solution was acidified to pH <2 with 4M hydrochloric acid and the precipitate was filtered off and recrystallised from ethanol to give 278 mg (20%) of the title compound; mp ca. 360° C. (decomposes gradually above 200° C.); 1H-NMR (DMSO-d6): δ1.68 (s, 6H), 7.12 (s, 1H), 7.17-7.41 (m, 6H), 10.72 (br s, 1H); MS: m/e 355/357 (M+); (C14H14ClN3O2S2) calc C, 47,25; H, 3.97; N, 11.81; found C, 46.82; H, 3.96; N, 11.62.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06329367B1 |
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| Source dataset | uspto-grants-2001_12 |
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| ORD ID | ord-59a66180165d4fde8c70363e11832e52 |
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| Source note | uspto-grants-2001_12 |
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