HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → HCID 72533160, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 72533163 | HCID 72533163 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 72533160 | HCID 72533160 | — |
Reaction Steps
To a solution of the (3R,9aS or 9aR)-3-{[(1,1-dimethylethyl)(dimethyl)silyl]methyl}octahydro-2H-pyrazino[1,2-a]pyrazine (D86, 217 mg) in 9 mL of dichloromethane was added triethylamine (212 μL) and it was brought to −10° C. A solution of acetyl chloride (54 μL) in 2 mL of dichloromethane was added dropwise. After 15 min the reaction was quenched by addition of MeOH. The crude was purified by flash chromatography (silica, CH2Cl2 to CH2Cl2: (0.5 M NH3 in MeOH) 95:5). The sample thus obtained was dissolved in CH2Cl2 and extracted with sat. NaHCO3. The organics were dried and the solvent removed, leading to the title compound (128 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07919491B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-f9e11cbbe2ad4209aeda8f7e060edc44 |
| Source note | uspto-grants-2011_04 |