Acetic Acid → 2,4-Diphenyl-6-(2-hydroxy-5-piperidinomethyl-4-hexyloxyphenyl)-s-triazine

HRID 1081455

Reaktionsgleichung

Reaktionsgleichung von HRID 1081455
[C:1]1([C:7]2[N:12]=[C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[N:10]=[C:9]([C:19]3[CH:24]=[CH:23][C:22]([O:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])=[CH:21][C:20]=3[OH:32])[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[N:33]1([CH2:39]N2CCCCC2)[CH2:38][CH2:37][CH2:36][CH2:35][CH2:34]1.[OH-].[Na+].C(O)(=O)C>C1(C)C=C(C)C=C(C)C=1.C1(C)C=CC=CC=1>[C:13]1([C:11]2[N:12]=[C:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[N:8]=[C:9]([C:19]3[CH:24]=[C:23]([CH2:39][N:33]4[CH2:38][CH2:37][CH2:36][CH2:35][CH2:34]4)[C:22]([O:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])=[CH:21][C:20]=3[OH:32])[N:10]=2)[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

Komponenten

7

Reaktionsbedingungen

Temperatur
160 °C

Versuchsvorschrift

2,4-Diphenyl-6-(2-hydroxy-4-hexyloxyphenyl)-s-triazine (42.5 g, 0.1 mol), dipiperidinomethane (17.5 g, 0.096 mol) and sodium hydroxide (0.8 g, 0.02 mol) are dissolved in 42 g of mesitylene. The mixture is heated with agitation at 160° C. for 18 hours. Acetic acid (8.5 g) is then added and the reaction mixture is heated for 30 minutes at 120°-130° C. Toluene (300 ml) is added and the heating is continued till the reaction product dissolves. The reaction mixture is then cooled to room temperature and the product crystallizes to give 21 g of reaction product. The crude product is recrystallized from 500 ml of toluene to yield 15 g of final product.

Aufarbeitung

  1. temperaturethe reaction mixture is heated for 30 minutes at 120°-130° C
  2. dissolutiondissolves
  3. temperatureThe reaction mixture is then cooled to room temperature
  4. customthe product crystallizes
  5. customto give
  6. custom21 g of reaction product
  7. customThe crude product is recrystallized from 500 ml of toluene

Quellen und Nachweise

ORD-Eintrag
ord-7ee19ae20808441c9ccaf60a2177e194
Quelldatensatz
uspto-grants-1996_12
Patentnummer
US05585422

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