HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 86628178, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | HCID 66617741 | HCID 66617741 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86628178 | HCID 86628178 | 154.7% |
Reaction Steps
Second step: To a stirred solution of carbonic acid ditrichloromethyl ester (triphosgene) (560 mg, 1.88 mmol) in CH2Cl2 (10 mL) at −78° C., was added a solution of (S)-1-methanesulfonyl-2-methyl-piperazine (838 mg, 4.70 mmol) and pyridine (0.74 mL, 9.4 mmol) in CH2Cl2 (10 mL) over 1 hour. The temperature was raised to RT, and stirring was continued over night. The organic phase was washed with H2O, dried over Na2SO4. Concentration under vacuo and flash chromatography (SiO2, EtOAc/H, 1:1) yielded 0.70 g (62%) of (S)-4-methanesulfonyl-3-methyl-piperazine-1-carbonyl chloride as a light yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08022099B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-00c9b2a34d404855a9275382ffdf3d7b |
| Source note | uspto-grants-2011_09 |