تفاعل #439289

معادلة التفاعل

product

4-Chloro-2-[[(1R)-4-iodo-1-phenylbutyl]oxy]benzonitrile

2-(ethylamino)ethanol

hydrogen chloride

→

title compound

المردود 65.4%

4-Chloro-2-[[(1R)-4-[ethyl(2-hydroxyethyl)amino]-1-phenylbutyl]oxy]-benzonitrile hydrochloride

المردود 65.4%

المذيبات

tetrahydrofuran

diethyl ether dichloromethane

diethyl ether

ظروف التفاعل

المعالجة

1. 1
   أخرىThe solvent was removed in vacuo
2. 2
   workup.DISSOLUTIONthe residue dissolved in water
3. 3
   استخلاصaqueous potassium carbonate and extracted with ethyl acetate (three times)
4. 4
   غسيلThe combined organic extracts were washed with water
5. 5
   تجفيفdried (Na2SO4)
6. 6
   أخرىevaporated
7. 7
   أخرىto give an oil
8. 8
   أخرىThe crystals that formed
9. 9
   أخرىwere collected
10. 10
    أخرىdried

الإجراء التجريبي

A solution of the product from Example 1 step (c) (200 mg) and 2-(ethylamino)ethanol (163 mg, 0.14 ml) in tetrahydrofuran (5 ml) was stirred for 2 days. The solvent was removed in vacuo and the residue dissolved in water and aqueous potassium carbonate and extracted with ethyl acetate (three times). The combined organic extracts were washed with water, dried (Na2SO4) and evaporated to give an oil. To a solution of this amine in diethyl ether-dichloromethane was added a 1M solution of hydrogen chloride in diethyl ether. The crystals that formed were collected and dried to afford the title compound as a white solid (65 mg). M.p. 141-144° C.

المصدر