반응 #74955

ord-65a73172a95d42a492af8ff8c50eb674

반응 조건

온도
45°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONis added, over 25 minutes
  2. 2
    workup.ADDITIONa mixture of 17 g (0.2 M)
  3. 3
    기타The desired product precipitates out at the end of the addition
  4. 4
    여과Filtration

실험 절차

To 73 ml dimethylformamide heated at 45° C. in which are dissolved 0.45 mole gaseous hydrochloric acid, is added, over 25 minutes, a mixture of 17 g (0.2 M) s.hexahydrotriazine of n. n.butylamine/and 26 g 2-(2-thienyl)ethylamine. The temperature of the medium is maintained at 45° C. throughout the addition by means of a cold water bath. The desired product precipitates out at the end of the addition. Filtration gives 22.16 g 4,5,6,7-tetrahydrothieno[3,2-c]pyridine hydrochloride (Yield: 65%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04174448uspto-grants-1979_11