HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 86628177, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | HCID 58006939 | HCID 58006939 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86628177 | HCID 86628177 | 178.8% |
Reaction Steps
Second step: To a stirred solution of carbonic acid ditrichloromethyl ester (triphosgene) (1.17 g, 3.95 mmol) in CH2Cl2 (20 mL) at −78° C., was added a solution of (R)-1-methanesulfonyl-2-methyl-piperazine (1.76 g, 9.9 mmol) and pyridine (1.60 mL, 20 mmol) in CH2Cl2 (20 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 1.70 g (71%) of (R)-4-methanesulfonyl-3-methyl-piperazine-1-carbonyl chloride as a light yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07812021B2 |
| Source dataset | uspto-grants-2010_10 |
| ORD ID | ord-ad6a2e5aa0844e1893eddac6528e246a |
| Source note | uspto-grants-2010_10 |