Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-Bromopropane-1-sulfonyl chloride | HCID 289329 | — |
| Reactant | HCID 67846374 | HCID 67846374 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 76488224 | HCID 76488224 | 72% |
Reaction Steps
A solution of Part A 3-bromopropyl sulfonyl chloride (1.06 g, 4.8 mmol) in dichloromethane (5 mL) was added dropwise to a cooled (-10° C.) stirred solution of Example 6a, Part B amine (1.05 g, 3.02 mmol) and triethyl amine (1.44 mL, 9.6 mmol) in dichloromethane (15 mL). After a few minutes, a precipitate formed. The suspension was stirred at -10° C. for 2.5 hours, diluted with dichloromethane (35 mL) and washed with 1N HCl solution (2×15 mL). The dichloromethane solution was dried (MgSO4), filtered and the solvent was removed in vacuo. The crude oil was purified on silica gel (Merck, 150 mL) eluting with 50% ethyl acetate in hexane to give title compound as a white foam (1.160 g, 72%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05741792 |
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| Source dataset | uspto-grants-1998_04 |
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| ORD ID | ord-eeedfc74393742b89ba7008c64e57f6a |
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| Source note | uspto-grants-1998_04 |
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