Ethylenediamine → Agn-PC-0niccc

반응식

[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:3]([CH2:10][C:11]#[N:12])=[N:2]1.[CH2:13](N)[CH2:14][NH2:15].C(=S)=S.C(Cl)(Cl)[Cl:21]>>[ClH:21].[NH:12]1[CH2:13][CH2:14][N:15]=[C:11]1[CH2:10][C:3]1[C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[O:1][N:2]=1

참가 물질

반응물 4

HCID 3301Ethylenediamine

HCID 6212Chloroform

HCID 6348Carbon Disulfide

HCID 3236401,2-Benzisoxazole-3-acetonitrile

생성물 1

HCID 12279087Agn-PC-0niccc

실험 절차

A mixture of 1,2-benzisoxazole-3-acetonitrile (1.6 g), ethylenediamine (0.7 g) and carbon disulfide (0.2 ml) was heated at 130° to 150°C for 0.5 hour and then allowed to stand at room temperature overnight. to the reaction mixture was added chloroform and the insoluble substance was filtered off. The filtrate was subjected to silica gel column chromatography and eluted with 10 to 20 % methanol-chloroform. The eluates were collected and treated with ethanolic hydrochloric acid to give the hydrochloride. The product was treated with charcoal and then recrystallized from ethanol to give the desired compound (0.4 g). m.p. 223° to 228°C.