HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,6-Lutidine → HCID 10480310, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,6-Lutidine | HCID 7937 | — |
| Reactant | Trimethyl orthoformate | HCID 9005 | — |
| Reactant | Cyclohexanemethylamine | HCID 76688 | — |
| Reactant | HCID 11858641 | HCID 11858641 | — |
| Reactant | Acetonitrile--water (1/1) | HCID 18373917 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 10480310 | HCID 10480310 | — |
Reaction Steps
To 180 mg of the previous crude material in 5 ml of dimethylformamide was added 0.15 ml of cyclohexylmethylamine together with 0.13 ml of trimethyl orthoformate and the reaction mixture was stirred for 24 hours at room temperature. After such time, 260 mg of 2-bromo-1-[2-(4-nitro-phenyl)-thiazol-4-yl]-ethanone was added together with 0.14 ml of 2,6-lutidine and the reaction mixture was stirred for another 24 hours at room temperature. After such time, 5 ml of a MeCN—H2O (1:1) solution is added to the reaction mixture, the precipitate is filtrated and washed with MeCN—H2O (1:1) and isopropylether to yield 264 mg of the title compound as a yellow solid, mp=184–187° C., MS (ISP) 481.3 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07135488B2 |
| Source dataset | uspto-grants-2006_11 |
| ORD ID | ord-6c07e17b166a409598e13e80488dac3a |
| Source note | uspto-grants-2006_11 |