HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 10706982, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 4-Bromo-3-methylaniline | HCID 23359 | — |
| Reactant | 3-Methyl-2-butenoyl chloride | HCID 102394 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10706982 | HCID 10706982 | 98.6% |
Reaction Steps
In accordance with Scheme 15, to the solution of 4-bromo-3-methyl-phenylamine (2 g, 1 eq.) in 5 mL of CH2Cl2 was added 10 mL of 2 M NaOH followed by dropwise addition of 3,3-dimethylacryloyl chloride (1.32 mL, 1.1 eq.) in 5 mL of CH2Cl2. The reaction was allowed to stir overnight and then partitioned between EtOAc and brine. The organic layer was separated, dried over Na2SO4, filtered and the solvent was removed in vacuo to afford 2.84 g (98.6%) of product Compound 53A as beige solid. Crude product was used for the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07638533B2 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-42a9b2b198404963a975487ed7c9c7b6 |
| Source note | uspto-grants-2009_12 |