반응 #1370862

ord-8d2503cbd24d4f42aa05e98aa44ae60a

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONA mixture of 13.7 g
  2. 2
    기타The oily product was partitioned into ether
  3. 3
    추출the ether mixture was extracted with 3N hydrochloric acid
  4. 4
    추출After extracting the acidic solution with methylene chloride, it
  5. 5
    추출re-extracted with methylene chloride
  6. 6
    건조The methylene chloride mixture, after water washing, drying
  7. 7
    농축concentrating in vacuo
  8. 8
    기타afforded 4.9 g

실험 절차

A mixture of 13.7 g. of triethylammonium furfuryldithiocarbamate, 10.5 ml. of methylene bromide, and 7.0 ml. of triethylamine in 100 ml. of dimethylformamide was stirred for several hours and then poured into ice-water. The oily product was partitioned into ether and the ether mixture was extracted with 3N hydrochloric acid. After extracting the acidic solution with methylene chloride, it was made basic with potassium hydroxide solution and re-extracted with methylene chloride. The methylene chloride mixture, after water washing, drying, and concentrating in vacuo afforded 4.9 g. of the desired dithietane as a yellow oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US03975528uspto-grants-1976_08