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ChemicalBook CAS DataBase List TETRAHYDRO-THIOPHEN-3-OL
3334-05-2

TETRAHYDRO-THIOPHEN-3-OL synthesis

3synthesis methods
-

Yield:3334-05-2 97%

Reaction Conditions:

with borane-THF in tetrahydrofuran at 5 - 20;

Steps:



Racemic 1 as an initial starting material for HPLC analysis was prepared as follows. Tetrahydrothiophene-3-one 2 (5.1g, 50mmol) was dissolved in THF (50mL) and cooled to 5°C. To this solution was added dropwise 1M BH3-THF (50mL, 50mmol) at 5°C, and the mixture was stirred overnight at room temperature. After monitoring that the reaction was complete by TLC (hexane/EtOAc 1:1), the reaction mixture was cooled again to 5°C, and MeOH (5mL) was slowly added at 5°C. Then, EtOAc (50mL) and 25% Rochelle salt solution (50mL) were added, and reaction mixture was vigorously stirred for 30min. The two layers were separated, and the aqueous layer was extracted with EtOAc (2×50mL). All organic layers were dried (Na2SO4), and evaporated in vacuum to yield racemic 1 (5.04g, 97%) as a colorless oil: 1H NMR (CDCl3, 500MHz) δ 4.63 (br s, 1H), 3.03-2.82 (m, 4H), 2.22-2.14 (m, 1H), 2.09 (d, J=6.0, 1H), 1.91-1.84 (m, 1H).

References:

Konuki, Kaname;Nagai, Hazuki [Tetrahedron Asymmetry,2014,vol. 25,# 24,p. 1581 - 1589]

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