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温度

0 °C

To a stirred suspension of 2,4-diamino-5-(2,3-dichlorophenyl)-6-hydroxymethylpyrimidine (185 mg; 1 mmol) in dry dichloromethane (25 ml), under nitrogen at -70° C., was added dropwise diethylaminosulphur trifluoride (263 μl; 2 mmol). The mixture was allowed to warm to 0° C. and kept at this temperature for 4 hours. After cooling to -70° C. the mixture was quenched with aqueous sodium bicarbonate, extracted with dichloromethane (2×50 ml), washed with saturated brine and dried (MgSO4). Concentration gave a colourless gum (0.2 g). Chromatography on silica gel, eluting with 0.01:1:19 Et3N:MeOH:CH2Cl2 gave the desired product which was triturated with CCl4 and dried in vacuo. 111 mg, mp. 224°-6° C.

1. temperatureAfter cooling to -70° C. the mixture
2. customwas quenched with aqueous sodium bicarbonate
3. extractionextracted with dichloromethane (2×50 ml)
4. washwashed with saturated brine
5. dry with materialdried (MgSO4)
6. concentrationConcentration