Hydrochloric Acid → 1,3-Dithiolane, 2-(m-tolyl)-

HRID 482779

반응식

HRID 482779 반응식
Cl.[CH3:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH:6]=O.[CH2:11]([SH:14])[CH2:12][SH:13]>C(Cl)(Cl)Cl>[CH3:2][C:3]1[CH:4]=[C:5]([CH:6]2[S:14][CH2:11][CH2:12][S:13]2)[CH:8]=[CH:9][CH:10]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric Acid3회HCID 109021,2-EthanedithiolHCID 121053-Methylbenzaldehyde

생성물 1

HCID 548731,3-Dithiolane, 2-(m-tolyl)-수율 71%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

Anhydrous HCl was bubbled rapidly for about 5 minutes through a solution of 46.87 gm (0.39 moles) of 3-methylbenzaldehyde and 44.92 gm (0.477 moles) of 1,2-ethanedithiol in 300 ml of CHCl3. During the addition of HCl, there was a slight exotherm with a rise in temperature to about 60° C. After completion of the addition of HCl, the reaction was stirred for 1 hour at room temperature, washed twice with 100 ml portions of water, dried with MgSO4, and fractionated to give 54.55 gm (0.278 moles) of a clear, colorless liquid (71% yield) b.p. 108°-110° C. (0.2 mm/Hg). Elemental analysis for C10H12S2 :

후처리

  1. customto about 60° C
  2. washwashed twice with 100 ml portions of water
  3. dry with materialdried with MgSO4

출처 및 근거

ORD 기록
ord-226d84cf1c8d423196290ebfe236b782
출처 데이터셋
uspto-grants-1986_03
특허 번호
US04575565

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