HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 13784631, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 13784630 | HCID 13784630 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 13784631 | HCID 13784631 | 55.6% |
Reaction Steps
To a suspension of 0.46 g of lithium aluminum hydride in 50 ml of ether was added dropwise, with ice-cooling, a solution of 1.6 g of 2-(3-ethoxycarbonylpropyl)-2H-1,4-benzothiazin-3(4H)-one in ether (30 ml). After the mixture was stirred for one hour, water was added dropwise thereto. The resultant white precipitates were filtered off, and the filtrate was dried (MgSO4). The solvent was evaporated off, and the residue was subjected to a column chromatography on silica-gel (70 g). From the eluate with hexane-ethyl acetate (1:1, v/v) was obtained 0.75 g (55.6%) of 2-(4-hydroxybutyl)-2H-1,4-benzothiazin-3(4H)-one. Recrystallization from ethyl acetate gave prisms, m.p. 101°-102° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04640916 |
| Source dataset | uspto-grants-1987_02 |
| ORD ID | ord-64106dae4adf4cc2b2c3433398b68704 |
| Source note | uspto-grants-1987_02 |