반응 #565309

반응 방정식

Potassium hydroxide

Methyl 3,5-dichloro-4-dodecyloxybenzoate

HCl

→

3,5-Dichloro-4-dodecyloxybenzoic acid

용매

THF

water

methanol

반응 조건

후처리

1. 1
   workup.ADDITIONadded to the solution
2. 2
   온도on gentle heating
3. 3
   workup.DISSOLUTIONdissolution
4. 4
   workup.STIRRINGwith good stirring whereupon the product
5. 5
   기타precipitated out
6. 6
   여과The white solid was filter off
7. 7
   세척washed well with water
8. 8
   기타air-dried
9. 9
   기타to remove as much of the water as possible
10. 10
    workup.STIRRINGstirred mechanically for about 1 hr
11. 11
    여과The solid was then filtered off
12. 12
    세척washed with acetonitrile
13. 13
    기타air-dried
14. 14
    기타Yield

실험 절차

Methyl 3,5-dichloro-4-dodecyloxybenzoate, (˜0.78 mol, as above) was dissolved in methanol (1000 mL) and THF (500 mL). 85%-Potassium hydroxide (100 g, 1.52 mol) was dissolved in water (200 mL) and added to the solution. The starting material oiled out, but on gentle heating dissolution was achieved. After stirring at room temperature for 15 minutes the solution was poured into ice cold 2N-HCl with good stirring whereupon the product precipitated out. The white solid was filter off, washed well with water, and air-dried to remove as much of the water as possible. The solid was then suspended in acetonitrile (˜1000 mL) and stirred mechanically for about 1 hr. The solid was then filtered off washed with acetonitrile and air-dried. Yield, 290.6 g.

출처