反应详情

温度

0 °C

Dissolve [2-benzothiazolyl][1-[2-(4-methoxyphenyl)ethyl]-4-piperidinyl]methanone (3.0 g, 7.88 mmol) in methanol (150 mL) and cool to 0° C. Add sodium borohydride (597 mg, 15.77 mmol) and stir for 1.5 hours, adding additional sodium borohydride after 30 minutes. Evaporate the solvent in vacuo and partition the residue between water and methylene chloride. Separate the organic phase, wash with saturated sodium chloride, dry (MgSO4) and evaporate the solvent in vacuo. Purify by recrystallization (ethyl acetate) to give the title compound as white fluffy crystals; mp 127°-129° C.

1. customEvaporate the solvent in vacuo
2. custompartition the residue between water and methylene chloride
3. customSeparate the organic phase
4. washwash with saturated sodium chloride
5. dry with materialdry (MgSO4)
6. customevaporate the solvent in vacuo
7. customPurify by recrystallization (ethyl acetate)