반응 #94720

반응 방정식

2-Amino-5-chloropyrimidine

methyl 2-(isocyanatosulfonyl)-benzoate

→

Methyl 2-{[(5-chloropyrimidin-2-yl)aminocarbonyl]-aminosulfonyl}benzoate

용매

methylene chloride

반응 조건

후처리

1. 1
   workup.ADDITIONto this was added
2. 2
   기타the desired product, 2-{[(5-chloropyrimidin-2-yl)aminocarbonyl]aminosulfonyl}benzoic acid, methyl ester, which had precipitated as a white solid
3. 3
   여과was filtered off

실험 절차

2-Amino-5-chloropyrimidine (1.3 g) was suspended in 20 ml of methylene chloride and to this was added with stirring 2.4 g of methyl 2-(isocyanatosulfonyl)-benzoate. After stirring for three hours at ambient temperature, the desired product, 2-{[(5-chloropyrimidin-2-yl)aminocarbonyl]aminosulfonyl}benzoic acid, methyl ester, which had precipitated as a white solid, was filtered off. It melted at 217°-221° and showed peaks in the nuclear magnetic resonance spectrum (trifluoroacetic acid solvent) at 4.0δ (singlet) for OCH3, 9.0δ for H at the 4- and 6-position of the hetero ring and at 7.9δ and 8.2-8.4δ for aromatic H, consistent for the above-named product.

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