Sodium Chloride → 2,4-Bis[(1-cyclohexyloxy-2,2,6,6-tetramethylpiperidin-4-yl)butylamino]-6-chloro-s-triazine

HRID 1587239ノート

反応式

HRID 1587239 の反応式
[C:1]([O:5]O)([CH3:4])([CH3:3])C.[Cl-].[Na+].[Cl:9][C:10]1[N:15]=[C:14]([NH:16][CH2:17][CH2:18][CH2:19][CH2:20][CH:21]2[CH2:26][C:25]([CH3:28])([CH3:27])[NH:24][C:23]([CH3:30])([CH3:29])[CH2:22]2)[N:13]=[C:12]([NH:31][CH2:32][CH2:33][CH2:34][CH2:35][CH:36]2[CH2:41][C:40]([CH3:43])([CH3:42])[NH:39][C:38]([CH3:45])([CH3:44])[CH2:37]2)[N:11]=1>[Mo](=O)(=O)=O.C1CCCCC1>[Cl:9][C:10]1[N:15]=[C:14]([NH:16][CH2:17][CH2:18][CH2:19][CH2:20][CH:21]2[CH2:26][C:25]([CH3:28])([CH3:27])[N:24]([O:5][CH:1]3[CH2:4][CH2:19][CH2:18][CH2:17][CH2:3]3)[C:23]([CH3:30])([CH3:29])[CH2:22]2)[N:13]=[C:12]([NH:31][CH2:32][CH2:33][CH2:34][CH2:35][CH:36]2[CH2:41][C:40]([CH3:43])([CH3:42])[N:39]([O:5][CH:1]3[CH2:4][CH2:22][CH2:21][CH2:20][CH2:3]3)[C:38]([CH3:45])([CH3:44])[CH2:37]2)[N:11]=1

参加物

6

反応物 3

HCID 5234Sodium ChlorideHCID 6410tert-Butyl hydroperoxideHCID 190733162-chloro-4,6-bis[N-(2,2,6,6-tetramethylpiperidin-4-yl)butylamino]-s-triazine

生成物 1

HCID 225076382,4-Bis[(1-cyclohexyloxy-2,2,6,6-tetramethylpiperidin-4-yl)butylamino]-6-chloro-s-triazine収率 74%

試薬・触媒・溶媒 2

HCID 14802Molybdenum trioxide触媒HCID 8078Cyclohexane溶媒

実験手順

A mixture of 57.7 g (0.448 mol) of 70% aqueous tert-butyl hydroperoxide, 250 ml of cyclohexane and 100 ml of saturated sodium chloride solution is agitated vigorously and the organic layer is then separated and dried over anhydrous magnesium sulfate. The drying agent is removed by filtration. The filtrate, 30.0 g (0.056 mol) of 2-chloro-4,6-bis[N-(2,2,6,6-tetramethylpiperidin-4-yl)butylamino]-s-triazine and 1.0 g of molybdenum trioxide are placed in a pressure bottle and heated at 130°-140° C. The reaction mixture quickly turns red and heating is continued till the red color is discharged. The reaction mixture is allowed to cool and solids are removed by filtration. The filtrate is concentrated under reduced pressure to give an oil which is purified by flash chromatography on silica gel to afford 30.3 g. (74% yield) of the title compound as a white glass.

後処理

  1. customthe organic layer is then separated
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customThe drying agent is removed by filtration
  4. temperatureheated at 130°-140° C
  5. temperatureThe reaction mixture quickly turns red and heating
  6. temperatureto cool
  7. customsolids are removed by filtration
  8. concentrationThe filtrate is concentrated under reduced pressure
  9. customto give an oil which
  10. customis purified by flash chromatography on silica gel
  11. customto afford 30.3 g

出典と根拠

ORDレコード
ord-267d377e12cb417cad4e97af0e519556
出典データセット
uspto-grants-1993_06
特許番号
US05216156

反応ノート

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