HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chlorobenzenesulfonyl chloride → HCID 67099968, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Chlorobenzenesulfonyl chloride | HCID 76187 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 67099219 | HCID 67099219 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67099968 | HCID 67099968 | 106% |
Reaction Steps
2-Chlorobenzene-1-sulfonyl chloride (301.9 mg, 1.43 mmol) was added to a solution of 2-(piperidin-4-ylmethyl)-6,7-dimethoxy-1,2,3,4-tetrahydroisoquinoline dihydrochloride (472 mg, 1.3 mmol) and N,N-diisopropylethylamine (1.3 ml, 7.5 mmol) in CH2Cl2 (25 mL) and the mixture was stirred overnight at room temperature. The resulting solution was washed with water (3×30 mL), dried over Na2SO4, and evaporated to dryness. The free base was dissolved in ethyl acetate (2 ml). A 2.8 M solution of hydrogen chloride in ethanol (0.6 mL) was then added. The product was crystallized and collected by filtration, and vacuum dried to give a white solid (406 mg, 63%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07928121B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-99a4212a931f4122835343d6bf09fdd8 |
| Source note | uspto-grants-2011_04 |