反应详情

To 186.3 g (4.9 mol) of sodium borohydride in 4 of tetrahydrofuran (THF) was added (over a 30 minute period 376 mL (4.9 mol) of trifluoroacetic acid TFA), with ice water cooling to maintain temperature below 15° C. [2R,3S]-2,3-bis(((1,1-Dimethylethyl)di-methylsilyl)oxymethyl)cyclobutanone-O-methyl oxime (400 g, 1.03 mol), from Step 2E, in 3 L of THF was added with ice water cooling to maintain the temperature below 20° C. After stirring the reaction mixture at ambient temperature overnight, it was concentrated, diluted with methylene chloride 3 L) and washed portionwise (with cooling with 400 mL of brine. After filtration, the layers of the filtrate were separated and the aqueous layer was washed with methylene chloride. The combined methylene chloride solution was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated to give crude title compound which was taken on to the next step without purification.

1. temperatureto maintain the temperature below 20° C
2. concentrationwas concentrated
3. additiondiluted with methylene chloride 3 L) and
4. washwashed portionwise (
5. temperaturewith cooling with 400 mL of brine
6. filtrationAfter filtration
7. customthe layers of the filtrate were separated
8. washthe aqueous layer was washed with methylene chloride
9. washThe combined methylene chloride solution was washed with brine
10. dry with materialdried over anhydrous magnesium sulfate
11. filtrationfiltered
12. concentrationconcentrated