HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86615024, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | HCID 68463627 | HCID 68463627 | — |
| Solvent | Oxolane--water (1/1) | HCID 21881883 | — |
| Product | HCID 86615024 | HCID 86615024 | 53% |
Reaction Steps
11.4 ml of hydrochloric acid (32%, excess) were added rapidly at 0° C. to a solution of 7-dimethylaminomethyl-8-(3-fluorophenyl)-1,4-dioxa-spiro[4.5]decan-8-ol hydrochloride (10.83 g, 31.3 mmol) in tetrahydrofuran/water mixture, and stirring was then carried out for 16 hours at RT. The mixture was adjusted to pH 11 with 32% sodium hydroxide solution, and extraction was carried out with ether. After evaporation of the solvent in vacuo, the residue was taken up in diisopropyl ether and EE, and the corresponding salt was precipitated by addition of methanesulfonic acid (1.88 ml, 28.9 mmol). 4.92 g (53%) of the product were obtained in the form of a colorless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07776848B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-e609beb641354455ab4ef8e6156de09a |
| Source note | uspto-grants-2010_08 |