HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 54463305, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,3-Dichlorobenzene-1-sulfonyl chloride | HCID 2734222 | — |
| Reactant | HCID 54221636 | HCID 54221636 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 54463305 | HCID 54463305 | 99.2% |
Reaction Steps
Triethylamine (0.63 ml) was added to a solution of (S)-4-(aminomethyl)-1-(7-bromo-1,4-benzodioxan-2-ylmethyl)piperidine (0.5 g) and 2,3-dichlorobenzenesulphonyl chloride (0.74 g) in dichloromethane (15 ml) and stirred under nitrogen for 24 hours. The reaction was diluted with dichloromethane (100 ml), washed with water (100 ml) and brine (100 ml), dried over anhydrous magnesium sulphate and concentrated under reduced pressure. Purification by flash chromatography on silica gel eluting with a 9:1 mixture of dichloromethane and methanol gave (S)-(-)-N-{[1-(7-bromo-1,4-benzodioxan-2-ylmethyl)-4-piperidyl]methyl}-2,3-dichlorobenzensulphonamide as a cream solid (0.8 g) m.p. 93-95° C., [α]D22 -37.1°(c=0.93, MeOH).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06136825 |
| Source dataset | uspto-grants-2000_10 |
| ORD ID | ord-7716a6aff3534ce9afbdb4711ce9d5e1 |
| Source note | uspto-grants-2000_10 |