Octylamine → 2-Octylamino-4-diisopropylamino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine

HRID 345992Notes

Reaction equation

HRID 345992 reaction equation
Cl[C:2]1[N:7]=[C:6]([N:8]([CH:12]([CH3:14])[CH3:13])[CH:9]([CH3:11])[CH3:10])[N:5]=[C:4]([N:15]2[C:20]([CH3:22])([CH3:21])[CH2:19][C:18]3([O:26][CH2:25][CH2:24][O:23]3)[CH2:17][C:16]2([CH3:28])[CH3:27])[N:3]=1.[CH2:29]([NH2:37])[CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36]>O>[CH2:29]([NH:37][C:2]1[N:7]=[C:6]([N:8]([CH:9]([CH3:10])[CH3:11])[CH:12]([CH3:13])[CH3:14])[N:5]=[C:4]([N:15]2[C:16]([CH3:27])([CH3:28])[CH2:17][C:18]3([O:26][CH2:25][CH2:24][O:23]3)[CH2:19][C:20]2([CH3:22])[CH3:21])[N:3]=1)[CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36]

Participants

4

Reactant 2

HCID 8143OctylamineHCID 199917752-Chloro-4-diisopropylamino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine

Product 1

HCID 199917982-Octylamino-4-diisopropylamino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

15 g (36.4 mmol) of the product from Example 18 are heated to 120° for 3 hours together with 30 ml of octylamine. After cooling, 40 ml of water are added and the mixture is extracted three times using 30 ml of methylene chloride. The CH2Cl2 solution is washed with water, dried over Na2SO4 and evaporated. The oily residue is dissolved in hexane/acetone and purified chromatographically on an SiO2 column. The main fraction is a viscous material.

Workup

  1. temperatureAfter cooling
  2. extractionthe mixture is extracted three times
  3. washThe CH2Cl2 solution is washed with water
  4. dry with materialdried over Na2SO4
  5. customevaporated
  6. dissolutionThe oily residue is dissolved in hexane/acetone
  7. custompurified chromatographically on an SiO2 column

Sources & evidence

ORD record
ord-321ec6453f6d406e908ab288eb00b8ed
Source dataset
uspto-grants-1991_10
Patent number
US05059689

Reaction notes

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