تفاعل #1536225

ord-a65b1e52956b49d791f297d92bb31817

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe mixture is heated
  2. 2
    درجة الحرارةto reflux for 4 hours
  3. 3
    workup.WAITThe mixture is then left
  4. 4
    درجة الحرارةto cool
  5. 5
    ترشيحfiltered over 10 g of aluminium oxide (activity I, neutral), which
  6. 6
    غسيلis back-washed with ether
  7. 7
    تركيزconcentrated in a vacuum
  8. 8
    workup.DISTILLATIONThe resulting crude product (9.5 g) is distilled through a Hempel column under a high vacuum

الإجراء التجريبي

A mixture of 8.26 g (0.052 mol) of 2-(4-methyl-5-thiazolyl)-ethyl-mercaptan and 33.07 g (0.208 mol) of dimethyldisulphide is treated with 50 mg of sodium hydride (50% dispersion in oil) and the mixture is heated to reflux for 4 hours. The mixture is then left to cool, filtered over 10 g of aluminium oxide (activity I, neutral), which is back-washed with ether, and concentrated in a vacuum. The resulting crude product (9.5 g) is distilled through a Hempel column under a high vacuum, there being obtained 6.45 g of [2-(4-methyl-5-thiazolyl)ethyl]-methyl-disulphide.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04188488uspto-grants-1980_02