HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 23366681, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 10130247 | HCID 10130247 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 23366681 | HCID 23366681 | — |
Reaction Steps
A solution of methanesulphonyl chloride (1.83 g) in dichloromethane (30 ml) was added dropwise at room temperature to a stirred solution of 6-fluoro-2,3,4,5-tetrahydro-1,4-benzothiazepine (2.65 g, prepared in a similar manner to its hydrochloride, Example 3 above) and triethylamine (1.6 g) in dichloromethane (60 ml). The reaction mixture was stirred at room temperature for 20 minutes, washed with water, dried and the solvent was removed by evaporation. Purification of the residue by flash chromatography using dichloromethane as eluent gave 6-fluoro-4-methylsulphonyl-2,3,4,5-tetrahydro-1,4-benzothiazepine, which was recrystallised from hexane. Yield 3.3 g (m.p. 115°-117° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05580866 |
| Source dataset | uspto-grants-1996_12 |
| ORD ID | ord-2af09b7658cf4699801752e4b4f7c52e |
| Source note | uspto-grants-1996_12 |