반응 #513851

반응 방정식

Myristic acid

aniline

→

Myristanilide

용매

xylene

—

denatured alcohol

반응 조건

후처리

1. 1
   기타A three liter flask equipped with a stirrer
2. 2
   기타nitrogen inlet, Barrett trap and condenser was used
3. 3
   온도heated for approximately 61/2 hours at a temperature of from about 170° C.-220° C
4. 4
   workup.ADDITIONpoured into a 4 liter beaker
5. 5
   여과the slurry of semi-solid myristanilide was collected by filtration
6. 6
   세척The filter cake was washed thoroughly with two portions of denatured alcohol
7. 7
   기타air dried at about 22° C

실험 절차

A three liter flask equipped with a stirrer, theremometer, nitrogen inlet, Barrett trap and condenser was used. Myristic acid (commercially available from Emery Chemicals, 97 percent purity, 685 grams, 3.0 moles), aniline (300 ml., 3.2 moles) and 120 ml xylene were charged to the flask. The mixture was stirred and heated for approximately 61/2 hours at a temperature of from about 170° C.-220° C. The reaction was conducted in a nitrogen atmosphere. The reaction mixture was then cooled to 140° C. and poured into a 4 liter beaker. About 1.8 liters of denatured alcohol were slowly added to the reaction solution. After standing overnight, the slurry of semi-solid myristanilide was collected by filtration. The filter cake was washed thoroughly with two portions of denatured alcohol and then air dried at about 22° C. The resultant white crystalline solid weighed 706 grams and had a melting point of 83.5° C.-84.5° C.

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