反应详情

Thionyl chloride (10.3 ml, 140.4 mmol) and N,N-dimethylformamide (one drop) were added to sodium 6-bromohexanesulfonate (5.00 g, 18.7 mmol) prepared by a process described in Org. Synth., Coll. Vol. II, 558 or WO95/19345 Pamphlet. The mixture was refluxed for 4 hours. The reaction mixture was concentrated in vacuo. The concentrate was diluted with benzene (50 ml). The resulting solution was washed twice with water (15 ml) and then with brine (10 ml), and thereafter dried over calcium chloride. The solvent was removed by evaporation in vacuo. Crude 6-bromohexanesulfonyl chloride (1.61 g) was obtained as a pale yellow oil.

1. customprepared by a process
2. temperatureThe mixture was refluxed for 4 hours
3. concentrationThe reaction mixture was concentrated in vacuo
4. additionThe concentrate was diluted with benzene (50 ml)
5. washThe resulting solution was washed twice with water (15 ml)
6. dry with materialwith brine (10 ml), and thereafter dried over calcium chloride
7. customThe solvent was removed by evaporation in vacuo