反応 #415527
ord-ae67ee17849d427b9f124b42b9e115c2
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1その他at from 10° to 12° C
- 2ろ過The reaction mixture is filtered
- 3洗浄washed with anhydrous benzene
- 4濃縮concentrated to a small volume
- 5ろ過filtered
- 6濃縮concentrated again to an oil which
実験手順
180 G. (1.23 moles) of 1-octanethiol and 97.2 g. (1.23 moles) of pyridine are added dropwise over one hour to 2000 g. of 12.5% phosgene in benzene maintaining the temperature at from 10° to 12° C with an ice water bath. The reaction mixture is allowed to warm to room temperature and stirred for 21 hours. The reaction mixture is filtered, washed with anhydrous benzene, concentrated to a small volume, filtered and concentrated again to an oil which infrared spectroscopy indicates is pure n-octylthiocarbonyl chloride.