تفاعل #583961

معادلة التفاعل

n-butylamine

butyrolactone

N-butyl-4-hydroxybutyramide

DIBAL

→

N-butyl-N-(4-hydroxybutyl)-amine

المذيبات

toluene

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto reflux under nitrogen atmosphere for 50 hours
2. 2
   أخرىVolatile solvents were removed in vacuo
3. 3
   درجة الحرارةThe solution was heated
4. 4
   درجة الحرارةAfter cooling to 0° C.
5. 5
   أخرىthe reaction was quenched with methanol (113 amount of DIBAL solution was used)
6. 6
   workup.ADDITIONfollowed by addition of saturated solution of Rochelle's salt
7. 7
   استخلاصThe mixture was extracted twice with EtOAc
8. 8
   غسيلthe organic extracts were washed with brine
9. 9
   تجفيفdried over Na2SO4

الإجراء التجريبي

A solution of 8.1 g (110 mmol) of n-butylamine and 8.6 g of butyrolactone in 50 ml toluene was allowed to reflux under nitrogen atmosphere for 50 hours. Volatile solvents were removed in vacuo. To a solution of 3.18 gm (20 mmol) of the resultant N-butyl-4-hydroxybutyramide in 50 ml of toluene were added 120 ml (120 mmol) DIBAL(25% W). The solution was heated with stirring at 70° C. for 18 hours. After cooling to 0° C., the reaction was quenched with methanol (113 amount of DIBAL solution was used) followed by addition of saturated solution of Rochelle's salt. The mixture was extracted twice with EtOAc; the organic extracts were washed with brine and dried over Na2SO4.

المصدر