反应详情

温度

0 °C

To a 25° C. solution of 1.0 g. (3.32 mmoles) of 3-[4-(1,1-dimethylheptyl)-2-hydroxyphenyl]-1,2,5,6-tetrahydropyridine in 15 ml. of acetonitrile is added 1.32 ml. (17.6 mmoles) of 37% formaldehyde solution. After stirring for one hour the reaction is cooled to 0° C. and 332 mg. (5.3 mmole) of sodium cyanoborohydride added. The reaction mixture is allowed to warm to 25° C. over a one hour period while the pH is maintained at 7 by the addition of acetic acid. The reaction mixture is evaporated, made basic with 2N potassium hydroxide and extracted with 200 ml. of dichloromethane. The organic extract is dried over magnesium sulfate and evaporated. The residue is crystallized from ether-pentane to yield 350 mg. of the title compound.

1. customTo a 25° C.
2. temperatureto warm to 25° C. over a one hour period while the pH
3. customThe reaction mixture is evaporated
4. extractionextracted with 200 ml
5. extractionThe organic extract
6. dry with materialis dried over magnesium sulfate
7. customevaporated
8. customThe residue is crystallized from ether-pentane
9. customto yield 350 mg