反応 #565309

反応方程式

Potassium hydroxide

Methyl 3,5-dichloro-4-dodecyloxybenzoate

HCl

→

3,5-Dichloro-4-dodecyloxybenzoic acid

溶媒

THF

water

methanol

反応条件

後処理

1. 1
   workup.ADDITIONadded to the solution
2. 2
   温度on gentle heating
3. 3
   workup.DISSOLUTIONdissolution
4. 4
   workup.STIRRINGwith good stirring whereupon the product
5. 5
   その他precipitated out
6. 6
   ろ過The white solid was filter off
7. 7
   洗浄washed well with water
8. 8
   その他air-dried
9. 9
   その他to remove as much of the water as possible
10. 10
    workup.STIRRINGstirred mechanically for about 1 hr
11. 11
    ろ過The solid was then filtered off
12. 12
    洗浄washed with acetonitrile
13. 13
    その他air-dried
14. 14
    その他Yield

実験手順

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.

出典