반응 #654562

반응 방정식

1,4-benzodioxan-6-amine

bis-(2-choroethyl)amine hydrochloride

potassium carbonate

→

1-(1,4-benzodioxan-6-yl) piperazine

수율 30.3%

용매

chlorobenzene

반응 조건

후처리

1. 1
   온도to reflux for 24 hours
2. 2
   기타The dark brown reaction mixture is then partitioned between 3N NaOH and methylene chloride
3. 3
   기타The organic layer is separated
4. 4
   건조dried over Mg2SO4
5. 5
   여과filtered
6. 6
   농축concentrated
7. 7
   기타Purification by flash column chromatography (8% methanol/methylene chloride on silica)

실험 절차

A solution of 1,4-benzodioxan-6-amine (2.00 g, 13.2 mmol), bis-(2-choroethyl)amine hydrochloride (3.54 g, 19.8 mmol) and potassium carbonate (1.83 g, 13.2 mmol) in of 20 mL chlorobenzene is heated to reflux for 24 hours. The dark brown reaction mixture is then partitioned between 3N NaOH and methylene chloride. The organic layer is separated, dried over Mg2SO4, filtered and concentrated. Purification by flash column chromatography (8% methanol/methylene chloride on silica) provides 0.88 g (30%) of the desired 1-(1,4-benzodioxan-6-yl) piperazine as a white solid (m.p. 138° C., TLC Rf 0.37 with 10% methanol/methylene chloride).

출처