Methanesulfonic Acid → HCID 18388784, Verbindung

HRID 279959

Reaktionsgleichung

Reaktionsgleichung von HRID 279959
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[N:9]1[N:13]=[C:12]2[CH:14]=[CH:15][CH:16]=[CH:17][C:11]2=[N:10]1.CS(O)(=O)=O.[CH2:23]=[CH:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30]>>[OH:1][C:2]1[C:7]([CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[N:9]1[N:13]=[C:12]2[CH:14]=[CH:15][CH:16]=[CH:17][C:11]2=[N:10]1

Komponenten

4

Edukt 3

HCID 6395Methanesulfonic AcidHCID 81251-Octene2×HCID 17113Drometrizole

Produkt 1

HCID 18388784HCID 18388784, Verbindung

Versuchsvorschrift

In a flask fitted with an nitrogen blanket, stirrer, reflux condenser and addition funnel, 225 grams of 2-(2-hydroxy-5-methylphenyl)-2H-benzotriazole, 65 ml of methanesulfonic acid and 156 ml of 1-octene are heated at 120° C. for a six-hour period. Throughout said period another 467 ml of 1-octene is added to the reaction mixture. The mixture is then cooled and extracted with two 200 ml portions of methanolic potassium hydroxide solution (40 grams potassium hydroxide in 100 ml of methanol). The extracts are washed with 1×400 ml and then with 4×200 ml of heptane. Water (200 ml) is added to the heptane extracts and the upper heptane layer is separated, washed with 5×200 ml of aqueous methanol (methanol 2:water 1). The washed heptane layer is dried over anhydrous magnesium sulfate and treated with 1×10 grams and then 1×5 grams of an acidic absorbent clay (FILTROL 13). After removal of the clay absorbent, the heptane solution is vacuum stripped at 110° C./2 mm to give 23 grams of the above-named product as a yellow liquid.

Aufarbeitung

  1. customIn a flask fitted with an nitrogen blanket, stirrer
  2. temperaturereflux
  3. additioncondenser and addition funnel
  4. waitThroughout said period
  5. temperatureThe mixture is then cooled
  6. extractionextracted with two 200 ml portions of methanolic potassium hydroxide solution (40 grams potassium hydroxide in 100 ml of methanol)
  7. washThe extracts are washed with 1×400 ml
  8. additionWater (200 ml) is added to the heptane extracts
  9. customthe upper heptane layer is separated
  10. washwashed with 5×200 ml of aqueous methanol (methanol 2:water 1)
  11. dry with materialThe washed heptane layer is dried over anhydrous magnesium sulfate
  12. additiontreated with 1×10 grams
  13. customAfter removal of the clay absorbent
  14. customstripped at 110° C.

Quellen und Nachweise

ORD-Eintrag
ord-45e64525b3214f35918f256da0561ab9
Quelldatensatz
uspto-grants-1986_05
Patentnummer
US04587346

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