تفاعل #829220

ord-97dc5b924a914ba985ae5b55c0017de1

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe reaction mixture is heated
  2. 2
    درجة الحرارةto reflux for 14 hours
  3. 3
    استخلاصextracted with diethyl ether
  4. 4
    استخلاصThe organic extract
  5. 5
    تجفيفis dried (MgSO4)
  6. 6
    ترشيحfiltered
  7. 7
    ترشيحThe resulting precipitate is filtered off

الإجراء التجريبي

A solution of tetrahydrothiopyran-4-one (4.64 g, 40.0 mmol) in methanol (10 mL) is added to a mixture of sodium cyanide (2.0 g, 40.0 mmol) and ammonium chloride (2.36 g, 44.0 mmol) in water (8 mL). The reaction mixture is heated to reflux for 14 hours. The mixture is diluted with water, basified with potassium carbonate, and extracted with diethyl ether. The organic extract is dried (MgSO4) and filtered. The solution is acidified with hydrochloric acid saturated with methylene chloride. The resulting precipitate is filtered off providing 4-amino-4-cyano-tetrahydrothiopyran hydrochloride salt.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05552419uspto-grants-1996_09