反応 #415527

ord-ae67ee17849d427b9f124b42b9e115c2

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他at from 10° to 12° C
  2. 2
    ろ過The reaction mixture is filtered
  3. 3
    洗浄washed with anhydrous benzene
  4. 4
    濃縮concentrated to a small volume
  5. 5
    ろ過filtered
  6. 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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04017505uspto-grants-1977_04