Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Ethanesulfonylchloride, 2-chloro- | HCID 15385 | — |
| Reactant | HCID 9815996 | HCID 9815996 | — |
| Reactant | HCID 86625994 | HCID 86625994 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68522192 | HCID 68522192 | — |
Reaction Steps
Chloroethane sulfonyl chloride (4.8 g, 0.029 mol) was added drop by drop to solution of 4-aminomethyl benzonitrile methan sulphonic acid salt acid (7 g, 0.029 mol) and pyridine (24 ml) in dry dichloromethane (25 ml) at −5° C. under nitrogen atmosphere. The reaction mixture was stirred at RT for 2 days and then partitioned between water and dichloromethane. The organic layer was washed with water and brine and dried over sodium sulfate. Solvent was evaporated under reduced pressure and the residue was purified by column chromatography over silica gel using 1% methanol in chloroform as eluent to give mixture of the sub-title compound and ethenesulfonic acid 4-cyano-benzylamide (3.4 g) as a solid. This was directly taken for next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07648985B2 |
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| Source dataset | uspto-grants-2010_01 |
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| ORD ID | ord-16776ca9a06f48358d16b8f3c4de1781 |
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| Source note | uspto-grants-2010_01 |
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