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

HRID 1081455

反応式

HRID 1081455 の反応式
[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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 7947Mesitylene溶媒

反応条件

温度
160 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7ee19ae20808441c9ccaf60a2177e194
出典データセット
uspto-grants-1996_12
特許番号
US05585422

関連ノート

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