HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 131736590, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 131736591 | HCID 131736591 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 131736590 | HCID 131736590 | 86.2% |
Reaction Steps
Compound 9A (5.5 g, 19 mmol) dissolved in DMF (15 ml) was added with K2CO3 (1.1 equiv., 2.75 g) and methyl iodide (1.1 equiv., 1.94 ml) and the reaction was stirred at rt overnight. The reaction was diluted with ethyl acetate and washed several times with water and finally with Brine. The organic phase was dried over sodium sulfate and concentrated under vacuum. The purification of the crude residue by crystallization from ethyl ether and petroleum ether afforded 5 g of 10A as a semisolid. Yield=86%. 1HNMR (DMSO, 200 MHz) δ 1.10 (3H, d, J=6.2 Hz), 2.94 (3H, s), 3.46 (3H, s), 4.22 (1H, q, J=6.4 Hz), 4.39 (1H, d, J=5.2 Hz), 5.16 (1H, d, J=3.2 Hz), 7.40 (2H, m), 7.82 (2H, m)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09409864B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-c23f02dea5db4654ae8a0061d6c4a9be |
| Source note | uspto-grants-2016_08 |