反应详情

13.76 g (44.8 mmol) of 8-bromo-THTMDBF obtained in Example 2 were added dropwise into a three-necked flask under nitrogen containing 1.31 g of magnesium and an iodine crystal in 5 ml of tetrahydrofuran, and the mixture was maintained under reflux for 2 h, 30 min. After the magnesium was filtered off, the reaction medium was poured into ice-cold water, acidified to pH 1 with concentrated hydrochloric acid and extracted with ether. The organic phase was washed with water, dried over magnesium sulfate, filtered and evaporated to yield 8.47 g (74%) of the expected compound, melting at 144.7° C.; αD =-7° (c=1, chloroform).

1. temperatureunder reflux for 2 h, 30 min
2. filtrationAfter the magnesium was filtered off
3. additionthe reaction medium was poured into ice-cold water
4. extractionextracted with ether
5. washThe organic phase was washed with water
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered
8. customevaporated