反应详情

温度

67.5 °C

2 M Lithium borohydride solutions (24.7 ml) was added to the flask under nitrogen atmosphere. Ethyl-2-(2-methoxytetrahydrofuran-3-yl)-2-oxoacetate (5 g) was dissolved in THF (25 ml) and slowly added at 65-70° C. Reaction mass was then maintained at 65-70° C. for 10 hrs. Reaction mass was cooled to −10° C. and slowly added concentrated hydrochloric acid (16 ml) and stirred for 2 hrs at −5 to 0° C. Triethyl amine (14.6 ml) was added to the reaction mass. Reaction mass was concentrated under vacuum. Ethyl acetate (20 ml) was added and again concentrated to residue. Ethyl acetate (50 ml) was added to it and filtered the un-dissolved salts. Filtrate was concentrated to get residue of Hexahydrofuro[2,3-b]furan-3-ol (yield 1.5 g).

1. additionslowly added at 65-70° C
2. customReaction mass
3. customReaction mass
4. temperaturewas cooled to −10° C.
5. customReaction mass
6. concentrationwas concentrated under vacuum
7. additionEthyl acetate (20 ml) was added
8. concentrationagain concentrated to residue
9. additionEthyl acetate (50 ml) was added to it
10. filtrationfiltered the un-dissolved salts
11. concentrationFiltrate was concentrated