HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → HCID 53328346, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | HCID 53328344 | HCID 53328344 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 53328346 | HCID 53328346 | 99.7% |
Reaction Steps
1.2 mL of acetyl chloride was slowly added to 10 mL of MeOH at 0° C. The solution was stirred for 30 min at room temperature and then tert-butyl N-{[3-methyl-2-(4-methylpiperazin-1-yl)-5-nitrophenyl]methyl}carbamate (300 mg, 0.82 mmol) dissolved in 5 mL of MeOH was added. The reaction mixture was stirred for 2 h and then evaporated. The residue was dissolved in 15 mL of water and washed with diethyl ether. The aqueous layer was made alkaline (pH=10) with an aqueous NaOH 1M and extracted with DCM. The combined organic layers were dried over Na2SO4, filtered and evaporated to yield expected compound as a pale yellow oil (216 mg, quantitative yield). m/z (ESI) 265.2 [M+H]+;
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08680095B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-64ae3cef29404b15a87e2e831fe43175 |
| Source note | uspto-grants-2014_03 |