HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thiomorpholine → HCID 9916982, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thiomorpholine | HCID 67164 | — |
| Reactant | HCID 18782110 | HCID 18782110 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 9916982 | HCID 9916982 | — |
Reaction Steps
To a solution of ~0.11 g of 4-[8-Chloro-3,7-dibromo-5,6-dihydro-11H-benzo[5,6 ]cyclohepta[1,2-b]pyridin-11-yl]-1-(chloroacetyl)piperidine in 5 ml of CH2Cl2 is added 0.12 ml of thiomorpholine and the mixture is stirred at ambient temperature for 24 h, and diluted with 20 ml of distilled water. The layers are separated and the aqueous layer is back extracted with 10 ml of CH2Cl2. The combined organic layer is washed once with saturated brine, dried over Mg2SO4, filtered and evaporated to a brown residue. Flash chromatography over 20 g silica gel with 200 ml of 3% MeOH/CH2Cl2 gives 0.12 g of the title compound, yield in two steps is 93.8%. MS: 614.5 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06071907 |
| Source dataset | uspto-grants-2000_06 |
| ORD ID | ord-fbd18b981bc34757b525ac74cc6a8bc4 |
| Source note | uspto-grants-2000_06 |