反応 #680500

ord-da3eba83bc83494aaff3409b0343bcb1

反応条件

温度
5°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was dripped into a reaction vessel
  2. 2
    workup.ADDITIONcontaining a mixed solvent
  3. 3
    抽出extraction
  4. 4
    その他the aqueous layer was removed
  5. 5
    洗浄the organic layer was washed with 180 g of water three times
  6. 6
    workup.DISTILLATIONAfter that, the solvent was distilled away

実験手順

Next, a mixed solution of bis(3-chloro-2-hydroxypropyl)disulfide described above and 250 g of methanol was dripped into a reaction vessel containing a mixed solvent consisting of 500 g of toluene and 240 g of 47% aqueous solution of sodium hydroxide with the temperature of the solution in the reaction vessel being maintained at 0 to 10° C. At the point of the completion, no scum-like insoluble matter was generated. 100 g of toluene was added to carry out extraction, the aqueous layer was removed, and the organic layer was washed with 180 g of water three times. After that, no scum-like insoluble matter was generated. After that, the solvent was distilled away, thereby obtaining 171 g of bis(β-epoxypropyl)disulfide.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09242947B2uspto-grants-2016_01