HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 10961937, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 10885591 | HCID 10885591 | — |
| Reactant | (Dimethyl sulfide)trihydroboron | HCID 12423031 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 10961937 | HCID 10961937 | 39% |
Reaction Steps
A stirred suspension of the product of Example 7 (85 mg, 0.17 mmol) in THF (9 mL) was heated to reflux and borane-methylsulfide (0.09 mL, 0.9 mmol) added. Stirring was continued for 3.5 h at reflux and overnight at room temperature. 6M HCl was added and the solution stirred for 2 h. The solution was applied to a Varian SCX column, washed with MeOH/CH2Cl2 50:50, then the product eluted with MeOH/CH2Cl2/NH4OH 50:50:1. The product was further purified on a silica column eluting with CH2Cl2/MeOH 98:2 to give the title compound 32 mg, 39%, mp 285-290° C.; MS (ES) 486,488 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06506769B2 |
| Source dataset | uspto-grants-2003_01 |
| ORD ID | ord-fd29e45de0794be18338437360146298 |
| Source note | uspto-grants-2003_01 |