반응 #549238

반응 방정식

dimethylformamide

Triethylamine

2-acetoxy-3-phenoxy-propylamine hydrochloride

trichloroacetamidine

→

N-(2-acetoxy-3-phenoxypropyl) trichloroacetamidine hydrochloride

용매

water

반응 조건

후처리

1. 1
   workup.ADDITIONmixture of 1.23 g
2. 2
   추출extracted with benzene
3. 3
   추출The benzene extract
4. 4
   세척is washed with water
5. 5
   건조dried over magnesium sulfate
6. 6
   여과filtered
7. 7
   농축concentrated
8. 8
   workup.DISSOLUTIONThe residue is dissolved in benzene
9. 9
   workup.ADDITIONtreated with an excess of ethanolic hydrogen chloride
10. 10
    농축Concentration to dryness

실험 절차

Triethylamine (0.50 g., 5.0 mmoles) is added in small portions over 10 minutes to a well stirred mixture of 1.23 g. (5.0 mmoles) of 2-acetoxy-3-phenoxy-propylamine hydrochloride and 1.61 g. (10 mmoles) of trichloroacetamidine in 5 ml. of dimethylformamide. The reaction mixture is heated at 60° C. for 2 hours, diluted with water and extracted with benzene. The benzene extract is washed with water, dried over magnesium sulfate, filtered and concentrated. The residue is dissolved in benzene and treated with an excess of ethanolic hydrogen chloride. Concentration to dryness affords N-(2-acetoxy-3-phenoxypropyl) trichloroacetamidine hydrochloride with a m.p. of 70° to 77° C.

출처