HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 86640248, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 86640249 | HCID 86640249 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86640248 | HCID 86640248 | 76% |
Reaction Steps
To a solution of 7-trityl-1,4,5,7-tetrahydro-1,6,7-triaza-as-indacene-2-carboxylic acid methyl ester XVII (1.1 mmol) in dry DMF (5 mL), NaH (2 eq) was added, the mixture was stirred at rt for 15 min then methyl iodide (2 eq) was added and the mixture was stirred at rt for 2 h. The mixture was poured into aq saturated NaH2PO4, extracted with AcOEt and the organic layer washed with water, dried (Na2SO4) and concentrated. The crude material was triturated with ethanol and filtered. Obtained the title compound (76% yield). ESI (+) MS: m/z 474 (MH+). 1H NMR (300 MHz): 2.48-2.59 (m, 1H), 2.62-2.92 (m, 3H), 3.79 (s, 3H), 3.89 (s, 3H), 6.44 (s, 1H), 7.11-7.31 (m, 15H), 7.61 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08207180B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-e57856a331b04b71898c2947fccf1b50 |
| Source note | uspto-grants-2012_06 |