Reaktion #884

Reaktionsgleichung

TS-2

water

TS-2

water

TS-1

water

TS-1

TS-2

4-hydroxy-(2'-ethylhexyl) benzoate

TS-2

→

4-hydroxy-nonyl benzoate

TS-2

Lösungsmittel

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturchill set
2. 2
   Sonstigeis used for melt preparation
3. 3
   workup.ADDITIONmixed with an aqueous gelatin solution
4. 4
   Sonstigeto give a crude dispersion
5. 5
   Temperaturchill set
6. 6
   Waschenwashed
7. 7
   Sonstigeto remove ethyl acetate
8. 8
   Temperaturchill set
9. 9
   Sonstigeuntil used for melt preparation
10. 10
    Sonstigeis obtained
11. 11
    Filtrationfilter
12. 12
    Sonstigeis combined with about 55.3 g of 8.3% (w/w) aqueous gelatin and 1.9 g of water at about 40° C.
13. 13
    workup.STIRRINGstirred
14. 14
    Temperaturchill set
15. 15
    Sonstigeis used for melt preparation
16. 16
    SonstigeThis roller milled dispersion

Vorschrift

A comparison thermal solvent dispersion 4-hydroxy-(2'-ethylhexyl) benzoate (TS-1), a liquid at room temperature, is prepared by similar means. An aqueous solution of 10% (w/w) aqueous DA-9 (6 g), 8.3% aqueous gelatin (about 54 g), and water (74.9 g) is combined with 15 g TS-1, stirred, passed through a colloid mill 5 times, chill set, and stored in the cold until it is used for melt preparation. This colloid milled dispersion is designated a TS-1 CM dispersion. A solid particle thermal solvent dispersion of 4-hydroxy-nonyl benzoate (TS-2; Pfaltz and Bauer; melting point 90°-93° C.) is prepared similarly. About 12 g of TS-2 was dissolved in 24 g of ethyl acetate and mixed with an aqueous gelatin solution comprising 4.8 g of 10% (w/w) aqueous DA-9, 43.3 g of 8.3% (w/w) aqueous gelatin, and 35.9 g of water to give a crude dispersion. This dispersion is passed through a colloid mill 5 times, chill set, noodled, washed to remove ethyl acetate, remelted, chill set, and stored in the cold until used for melt preparation. This colloid milled dispersion is designated TS-2 (CM). Another solid particle thermal solvent dispersion of TS-2 is prepared by roller milling methods. About 18 g of TS-2 is combined with 36 g of 10% aqueous DA-9 , 66 g of water, and about 100 mL of 1.8-2.1 mm-diameter zirconia milling media and placed in a sealed glass jar. This jar is placed on a roller mill for about 123 hours, and a fine particle sized aqueous dispersion is obtained. This dispersion is passed through a cloth filter. About 110 g of this filtrate is combined with about 55.3 g of 8.3% (w/w) aqueous gelatin and 1.9 g of water at about 40° C., stirred, chill set, and stored in the cold until it is used for melt preparation. This roller milled dispersion is designated TS-2 RM.

Quelle