HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → HCID 66618321, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 86636735 | HCID 86636735 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66618321 | HCID 66618321 | 93% |
Reaction Steps
To (S)-2-Amino-3-p-tolyl-propionic acid cyclopentyl ester p-toluenesulfonic acid salt prepared in the above stage (10 g, 0.022 mol) was added dichloromethane 200 ml) under nitrogen. Triethylamine (6.29 ml, 0.044 mol) was added dropwise with stirring. Acetyl chloride (1.72 ml, 0.022 mol) in dichloromethane (50 ml) was added dropwise to the reaction. Acetyl chloride (0.1 ml) in DCM (0.5 ml) was added after 20 mins and the reaction reached completion after 1 hr. The organic phase was washed with saturated sodium bicarbonate (3×200 ml), dried (Na2SO4) and the solvent removed in vacuo. The required product was obtained 6.62 g, 93% yield and was used in the next step without further purification. m/z 321 [M++H]+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07973181B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-6fc2039d94784ce58589f47fd7320d9b |
| Source note | uspto-grants-2011_07 |