HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzenesulfonyl chloride → HCID 11539725, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzenesulfonyl chloride | HCID 7369 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 86631061 | HCID 86631061 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 11539725 | HCID 11539725 | — |
Reaction Steps
To a vigorously stirred solution/suspension of the product from example 69 part f) (0.393 g) and solid sodium bicarbonate (0.342 g) in DCM (3 ml) and water (3 ml) was added benzenesulfonyl chloride (0.21 ml) dropwise. The mixture was stirred for 16 h. The organic layer and 1 further DCM extract were combined and purified by passage through SCX resin eluting with MeCN, MeOH followed by 7M NH3 in MeOH. The basic fractions were concentrated in vacuo, dissolved in DCM (3 ml) and treated with TFA (20 ml) for 16 h. Concentration in vacuo and purification by RPHPLC gave the title product as a white foam (45 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08524715B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-d51f154a50e04dda8f7fec84464bd025 |
| Source note | uspto-grants-2013_09 |