反应详情

The hydroxymethyl compound (4.84 g; 0.02 mole) prepared in (a) above, was dissolved in dimethylformamide (30 ml) cooled to 0°-5° C. and thionyl bromide (1.7 ml; 0.02 mole) was added dropwise with stirring. After 2 hours the greenish-yellow solution was poured onto ice/water and extracted via diethyl ether. The ether extract was washed with NaCl (saturated solution) dried over molecular sieve 3A and evaporated to give a light brown oil which slowly crystallised (4.6 g).

1. temperaturecooled to 0°-5° C.
2. additionAfter 2 hours the greenish-yellow solution was poured onto ice/water
3. extractionextracted via diethyl ether
4. extractionThe ether extract
5. washwas washed with NaCl (saturated solution)
6. dry with materialdried over molecular sieve 3A
7. customevaporated
8. customto give a light brown oil which
9. customslowly crystallised (4.6 g)