HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 10H-Pyrazino[2,3-b][1,4]benzothiazine-8-methanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | methyl 10H-pyrazino[2,3-b][1,4]benzothiazine-8-carboxylate | HCID 11747308 | — |
| Reactant | Lithium aluminum lithium hydride | HCID 18670308 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 10H-Pyrazino[2,3-b][1,4]benzothiazine-8-methanol | HCID 10944292 | 70.1% |
Reaction Steps
Into a solution of 40 g of lithium aluminum lithium hydride in tetrahydrofuran (1 l) was dropped a solution of 200 g of methyl 10H-pyrazino[2,3-b][1,4]benzothiazine-8-carboxylate in tetrahydrofuran (2.5 l) while maintaining the mixture at a temperature not exceeding 15° C. After continuing the reaction at 15° C. or below for 1 hour, 40 ml of water, 40 ml of a 15% aqueous solution of sodium hydroxide and 120 ml of water were successively added and the resulting mixture was stirred for an additional 1 hour. After filtering off the insoluble matter, the solvent was distilled off under reduced pressure to thereby give 125 g of the title compound as yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06518423B1 |
| Source dataset | uspto-grants-2003_02 |
| ORD ID | ord-0ea0ec49df8b4a38b307025b56fa3dcc |
| Source note | uspto-grants-2003_02 |