반응 #63335

반응 방정식

3-[3-[1-Piperidinylmethyl]phenoxy]propanamine

N-cyano-1-methyl-2-(phenylmethylene) hydrazine carboximidothioic acid, methyl ester

hydrochloric acid

→

title compound

수율 28.5%

1-Methyl-N5 -[3-[3-[1-piperidinylmethyl]phenoxy]propyl]-1H-1,2,4-triazole-3,5-diamine

수율 28.5%

용매

Acetone

반응 조건

후처리

1. 1
   세척washed with ether
2. 2
   추출extracted with ethyl acetate
3. 3
   기타Evaporation of the ethyl acetate
4. 4
   기타crystallised from toluene/ether

실험 절차

3-[3-[3-[1-Piperidinylmethyl]phenoxy]propanamine (2.48 g) and N-cyano-1-methyl-2-(phenylmethylene) hydrazine carboximidothioic acid, methyl ester (2.32 g) were heated at 70° under water-pump vacuum for 4 hr. Acetone was added and the solution was treated with dilute hydrochloric acid for 1 hr, washed with ether, basified and extracted with ethyl acetate. Evaporation of the ethyl acetate extracts fgave an oil which crystallised from toluene/ether to give the title compound as a white solid (0.98 g) m.p. 94°-5°. TLC silica, methanol/0.88 ammonia 80:1, Rf 0.5.

출처