HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 70160832, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 70161439 | HCID 70161439 | — |
| Solvent | Sulfuric Acid | HCID 1118 | — |
| Product | HCID 70160832 | HCID 70160832 | 96.4% |
Reaction Steps
(Z)-4,4-Difluoro-5-[2-(4-methylpiperazin-1-yl)-2-oxoethylidene]-1-tosyl-2,3,4,5-tetrahydro-1H-1-benzoazepine (11.7 g) was dissolved in 20 ml of concentrated sulfuric acid, followed by stirring for 24 hours at room temperature. The reaction solution was poured over 700 ml of a 1N aqueous solution of sodium hydroxide and extracted with chloroform. The organic layer was washed with a saturated aqueous solution of NaCl, and after drying over magnesium sulfate, the solvent was evaporated off. The resulting residue was crystallized from diethyl ether to give 7.62 g of (Z)-4,4-difluoro-5-[2-(4-methylpiperazin-1-yl)-2-oxoethylidene]-2,3,4,5-tetrahydro-1H-1-benzoazepine as a colorless powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06340678B1 |
| Source dataset | uspto-grants-2002_01 |
| ORD ID | ord-efc95f98c2d34343b53550df0de868ae |
| Source note | uspto-grants-2002_01 |