HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 59822278, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | HCID 67336483 | HCID 67336483 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 59822278 | HCID 59822278 | — |
Reaction Steps
Dissolve 7-chloro-6-(1H-imidazol-2-ylthiomethyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine hydrochloride (9.85 g, 29.85 mmol) in water (60 mL) and absolute ethanol (40 mL) in a flask. Add a solution of Na2CO3 (15.8 g, 149 mmol) in water (100 mL) followed by DCM (125 mL) to the flask. Stir the mixture vigorously, then separate layers. Extract the aqueous layer twice with a solution of DCM (100 mL) and ethanol (10 mL). Dry the combined organic extracts over Na2SO4. Filter and concentrate in vacuo to obtain 7-chloro-6-(1H-imidazol-2-ylthiomethyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine as a light yellow foam (7.4 g, 75% weight recovery). MS (APCI+) m/z: 294.25 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07994163B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-cf21b55e063a4577b20af9d8cf6b3744 |
| Source note | uspto-grants-2011_08 |