반응 #322204

반응 방정식

ethyl-2-cyano-2-(2,3-dichlorophenyl)acetate

sodium

guanidine hydrochloride

Sodium

→

title compound

2,4-Diamino-5-(2,3-dichlorophenyl)-6-hydroxypyrimidine

용매

ethanol

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   온도The mixture was refluxed for 8 hours
3. 3
   기타EtOH was removed under reduced pressure
4. 4
   기타the residue was partitioned between EtOAc and water
5. 5
   추출The EtOAc layer was extracted with 2N NaOH
6. 6
   온도with cooling
7. 7
   여과The precipitated solid was filtered
8. 8
   기타dried

실험 절차

Sodium (1.2 g, 0.052 mol) was added in portions to absolute ethanol (50 ml) with stirring. After the sodium had dissolved guanidine hydrochloride (3.69 g, 0.039 mol) was added followed by ethyl-2-cyano-2-(2,3-dichlorophenyl)acetate (5 g, 0.0195 mol). The mixture was refluxed for 8 hours, EtOH was removed under reduced pressure and the residue was partitioned between EtOAc and water. The EtOAc layer was extracted with 2N NaOH and the extract was neutralised with 2N HCl with cooling. The precipitated solid was filtered and dried to give the title compound. (0.22 g), mp. 275° C. (decomp). Microanalysis: Calcd: for 0.25 hydrate: C, 43.56; H, 3.09; N, 20.33; C, 43.76; H, 3.09; N, 20.03.

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