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

HRID 1081455

반응식

HRID 1081455 반응식
[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

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 70151DipiperidinomethaneHCID 49927612-(2-Hydroxy-4-hexyloxyphenyl)-4,6-diphenyl-1,3,5-triazine

생성물 1

HCID 1358111922,4-Diphenyl-6-(2-hydroxy-5-piperidinomethyl-4-hexyloxyphenyl)-s-triazine수율 29.9%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 7947Mesitylene용매

반응 조건

온도
160 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7ee19ae20808441c9ccaf60a2177e194
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05585422

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