Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 21841970 | HCID 21841970 | — |
| Reactant | HCID 21841981 | HCID 21841981 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 88308980 | HCID 88308980 | — |
Reaction Steps
To a solution of 25 mL of N,N-dimethylformamide containing 0.11 g of the title compound of Step D under a nitrogen atmosphere was added 0.17 g of potassium carbonate and 0.11 g of 3-chloro-7-methoxy-1,2,4-benzotriazine 1-oxide. The reaction mixture was stirred at room temperature for approximately 24 h, and was then poured into water and extracted with dichloromethane. The organic extracts were washed with water and saturated aqueous sodium chloride. The organic layer was dried over magnesium sulfate, filtered and the filtrate was then evaporated to obtain a yellow oil. The yellow oil was crystallized from 1-chlorobutane/hexane to yield 0.11 g of the title compound of Step E, a compound of the invention, as a yellow solid melting at 191-192° C. 1H NMR (400 MHz, CDCl3): δ 3.250 (s,3H), 3.827 (s,3H), 3.964 (s,3H), 7.4-7.52 (m,5H), 7.65 (d,1H), 7.723 (d,1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05962436 |
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| Source dataset | uspto-grants-1999_10 |
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| ORD ID | ord-5e8267c8c51b47cb9302aa41399b025e |
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| Source note | uspto-grants-1999_10 |
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