HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 66722397, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 58117543 | HCID 58117543 | — |
| Product | HCID 66722397 | HCID 66722397 | — |
Reaction Steps
Under a nitrogen atmosphere 1.7 g (12.3 mmol) 1-chloroethyl chloroformiate was added to 2.0 g (8.2 mmol) 6-benzyl-5,6,7,8-tetrahydro-4H-thiazolo[4,5-d]azepine (CAS Registry Number: 1159094-24-2) in 20 mL DCM at 0° C. The reaction mixture was stirred at RT for 2 h. The reaction mixture was concentrated and 20 mL anhydrous methanol was added. The reaction mixture was stirred under reflux for 1 h and concentrated. The resulting crude product was washed with DCM, the solid was filtered and dried. Yield: 0.35 g (58% of theory). ESI-MS: m/z=199 (M+H)+; Rt(HPLC): 0.52 min (Method J).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09029360B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-ca6e7573d38b48038420baae223e5aec |
| Source note | uspto-grants-2015_05 |